Synthesis,Structure and Luminescent Properties of [Zn（btzb）2Cl2]·2H2O [btzb = 1,2-Bis（5-tetrazolyl）benzene]

The title compound [Zn（btzb）2Cl2]·2H2O （1·2H2O, btzb = 1,2-bis（5-tetrazolyl）ben- zene） was synthesized in situ by the [2＋3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions. 1·2H2O crystallizes in the monoclinic system, space group P2 1/c with a = 9.0119（18）, b = 7.5566（15）, c = 18.076（5）A, β= 114.67（2）°, V= 1118.6（4）A^3, Z = 2, Dc = 1.784 g/cm^3, T= 223（2） K, C16H16N16O2Cl2Zn, Mr = 600.74, F（000） = 608, μ（MoKα） = 1.393 mm^-1, S = 1.081, R = 0.0306 and wR = 0.0669 for 1896 observed reflections with I 〉 2σ（I）. The Zn^2＋ ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms, forming a distorted octahedral coordination geometry. A number of intermolecular hydrogen bon- ding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure. The luminescent property of 1·2H2O was also investigated.     

Hydrothermal Synthesis,Crystal Structure and Electrochemical Properties of a New Dinuclear Copper Complex [C2H6ON]2[Cu2Cl2（μ-CH3COO）4]

The hydrothermal reaction of copper chloride dihydrate and 5,5-dimethyl-imidazolidine,-2,4-dione with a mole ratio of 1：1 in acetonitrile resulted in the formation of a new acetate-bridged dinuclear copper complex, [C2H6ON]2[Cu2Cl2（μ-CH3COO）4]. Protonated acetamide in eaolie form and acetic acid were yielded by the hydrolysis of acetonitrile under hydrothennal condition. The rifle complex （C12H24Cl2Cu2N2O10） was characterized by X-ray single-crystal diffraction, IR spectrum, elemental and electrochemical analysis. It crystallizes in the monoclinic system, space group P21/c with a = 8.298004）, b = 14.358（2）, c = 12.0010（2） A^°, β= 130.620（3）°, V = 1085.3（2） A^°^3, Dc = 1.696 g/cm^3, 34, = 554.31, Z = 2, F（000） = 564 and μ = 2.254 mm^-1. The crystal structure consists of a tetraacetate-bridging dinulcear copper complex anion [Cu2Cl2（μ-CH3COO）4]^2-, with the chlorine anions in the axial positions, and two protonated acetamide cations [C2H6ON]^＋, which were connected through hydrogen bonds to form a three-dimensional infinite network.     

Synthesis and Crystal Structure of a Distorted 2D （6,3） Layer Complex, [Cd（H2mbdpz）（N3）2]n （H2mbdpz = 4,4′-Methylenebis（3,5-dimethylpyrazole）） Containing both End-on and End-to-end Azide Bridges

The complex [Cd（H2mbdpz）（N3）2]n 1 （H2mbdpz = 4,4′-methylenebis（3,5-dimethylpyrazole）） has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in the monoclinic system, space groups C2/c with a = 22.154（5）, b = 7.4835（15）, c = 21.044（8）A^°,β= 115.51（3）°, V= 3148.7（17）A^°3, Z= 8, C11H16CdN10, Mr = 400.75, Dc = 1.691 g/cm^3,μ = 1.401 mm^-1, F（000） = 1599, T= 293（2） K, the final R = 0.0228 and wR = 0.0581 for 3604 observed reflections with I 〉 2σ（I）. The structural determination revealed that the coordination environment of Cd（Ⅱ） atom is a distorted octahedron consisting of two nitrogen donors of two H2mbdpz ligands and four nitrogen donors from four azide ligands. The azide moieties act as bridges in two modes： end-on （μ1,1-） and end-to-end （μ1,3-）, and H2mbdpz also serves as a bridge with a bis-monodentate coordination. Both bridging ligands link the Cd（Ⅱ） atoms to form a distorted two-dimensional （6,3） layer.     

Synthesis,Crystal Structure and Photoluminescent Properties of a New Dinuclear Copper（Ⅰ） Complex [Cu2（μ2-dppm）2（MeCN）2（μ2-MeCN）]（ClO4）2·MeCN

The title compound [Cu2（μ2-dppm）2（MeCN）2（μ2-MeCN）]（ClO4）2·MeCN （dppm = bis（diphenylphosphino）methane） has been prepared and characterized. It crystallizes in the monoclinic system,space group P21/n,with a = 11.904（6）,b = 20.755（11）,c = 24.744（13）A,β = 98.226（12）°,C58H56Cl2Cu2N4O8P4,Mr = 1258.93,V = 6051（5） A^3,Z = 4,Dc = 1.382 g/cm^3,μ = 9.52 mm^-1,F（000） = 2592,R = 0.0533 and wR = 0.1295 for 6175 observed reflections with I 〉 2σ（I）. Each Cu（I） center is tetrahedrally coordinated by two phosphine atoms from two bridging dppm ligands,one nitrogen atom from a terminally coordinated acetonitrile molecule,and another nitrogen atom from a μ2-acetonitrile molecule. The two Cu（I） centers are bridged by two dppm ligands as well as a unique acetonitrile molecule. The full molecule exhibits a ＇chair-like＇ configuration. This dinuclear complex exhibits intense or middle photoluminescence at room temperature in the solid state or actonitrile solution at 486 nm.     

A Layered Vanadium Oxide with Cobalt（Ⅱ） Coordination Complex： Hydrothermal Synthesis and Crystal Structure of （py）5Co2（H2O）3[V4O12]

A novel layered mixed metal vanadium-cobadt complex, （py）5Co2（H2O）3[V4O12] 1 （py = pyridine）, was hydro（solvo）thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group Pca21 with a = 17.473（4）, b = 11.447（2）, c = 17.509（4）A^°, V = 5005.3（7）A^°3, Z = 4, Mr = 3502.1（12）, Z = 4, Dc = 1.827 g/cm^3,μ（MoKα） = 2.023 mm^-1, F（000） = 1928, S = 1.020, the final R = 0.0400 and wR= 0.1063 for 6035 observed reflections with I 〉 2σ（I） and 460 variables. Complex 1 consists of tetrahedral VO4 groups to form the large layers which are alternately bonded by two cobalt complex species Co（py）2（H2O）2 and Co（py）3（H2O）.     

Syntheses and Crystal Structures of Two New Organically Templated Borates： [（C2H10N2）]2[B14O20（OH）6] and [C8H22N4][B5O6（OH）4]2

Two new nonmetal borates, [（C2H10N2）]2[B14O20（OH）6] 1 and [C8H22N4][B5O6（OH）4]2 2, have been synthesized under mild conditions and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis and thermogravimetric analysis. Crystal data for compound 1： triclinic, space group P^-1, a = 8.4979（17）, b = 8.8498（18）, c = 10.065（2）A^°, α = 95.01（3）, β = 96.99（3）, γ = 116.82（3）°, V= 661.8（3）A^°^3, Z= 1, Mr = 697.63, Dc = 1.751 g/cm^3,μ = 0.163 mm^-1, F（000） = 356, the final R = 0.0372 and wR = 0.0968 （I 〉 2σ（I））; and those for compound 2： monoclinic, space group P21/c, a = 9.1867（18）, b= 14.118（3）, c = 10.334（2）A^°, β = 91.48（3）°, V = 1339.8（5）A^°^3, Z = 2, Mr = 610.46, Dc = 1.513 g/cm^3,μ = 0.135 mm^-1, F（000） = 632, the final R = 0.0350 and wR = 0.0912 （I 〉 2σ（I））. For both 1 and 2, the anionic units are interlinked via O-H…O hydrogen bonds to form a 3D supramolecular network, while the protonated cations are located in the free space of the inorganic borate framework and interact with the anions by electrostatic attraction and extensive N-H…O hydrogen bonds.     

Synthesis and Crystal Structure of a New Mo/Au/S Cluster [Et4N][Mo2S4（AuPPh3）（edt）2]· 0.25Et2O·0.25MeOH （edt = Ethanedithiolate）

Reactions of the preformed cluster precursor [Et4N]2[Mo2S2（μ-S）2（edt）2] （edt = ethanedithiolate） （1） with [Au（PPh3）Cl] in MeOH/MeCN gave rise to a new heterobimetallic Mo/Au/S cluster [Et4N][Mo2S4（AuPPh3）（edt）2]·0.25Et2O·0.25MeOH （2·0.25Et2O·0.25MeOH）. It was characterized by elemental analysis, IR spectrum and X-ray analysis. 2·0.25Et2O·0.25MeOH crystallizes in the monoclinic system, space group C2/c with a = 20.117（4）, b = 9.2705（19）, c = 44.418（9） A^°, β= 93.19（3）°, V = 8271（3） A^°^3, Z = 8, Dc = 1.794 g/cm^3, T = 193 K, C31.25H43AuMo2NO0.50PS8, Mr = 1116.96, F（000） = 4380, μ（MoKa） = 4.603 mm^-1, S = 1.019, R = 0.0672 and wR = 0.1708 for 7243 observed reflections with I 〉 2σ（I）. The anion of 2 consists of a butterfly-shaped Mo2S4Au core in which one [AuPPh3]^＋ cation is coordinated by one bridging S and two terminal S atoms of the [（edt）2Mo2（S）2（μ-S）2] moiety. The Au（I） center adopts a pseudo-tetrahedral coordination geometry, and the Au-S bond lengths vary from 2.425（2） to 2.898（3）A^°.     

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 ofa Bipy Bridged Binuclear Cu^Ⅱ Complex Containing Aminomethanesulfonic Acid [Cu2（Sams）2（Bipy）（H2O）2]·（H2O）

The title complex [Cu2（Sams）2（H2O）2（bipy）]·（H2O） 1 （H2Sams = N-（2-hydroxybenzy） aminomethanesulfonic acid, bipy = 4,4′-bipyridine） has been synthesized by the reaction of Cu- （CH3COO）2·H2O, nESams and 4,4′-bipyridine in aqueous methanol. It was characterized by IR, elemental analysis, thermogravimetric analysis （TGA） and X-ray diffraction analysis. Complex 1 crystallizes in monoclinic, space group P21/n with a= 10.9533（17）, b = 8.3408（13）, c = 16.714（3） A^°, β = 101.295（4）°, V = 1494.3（4） A^°3 and Z = 2. The asymmetric unit is comprised of a tridentate Schiff base Sams^2- anionic ligand, a 4,4′-bipyddine and two coordinated water molecules, thus forming a binuclear copper（Ⅱ） complex. The coordination environment at Cu^Ⅱ center is described as a slightly distorted square pyramidal geometry. Via intermolecular hydrogen bonds C（10）-H（10）…O（3） and C（13）- H（13）…O（3）, an infinite supramolecular chain is yielded. A number of intermolecular hydrogen bonds greatly contribute to the stabilization of the solid-state structure for 1.     

Syntheses and Structures of Two New Cobalt Supramolecular Complexes, [Co（4,4＇-bipy）2（H2O）4]·[Co2（4,4＇-bipy）3（H2O）8]·2TST·2（4,4＇-bipy）·4H2O and [Co（4,4＇-bipy）2（H2O）4]DSNT·4,4＇-bipy

Two new cobalt（II） supramolecular complexes [Co（4,4＇-bipy）2（H2O）4]·[Co2（4,4＇-bipy）3（H2O）8]·2TST·2（4,4＇-bipy）·4H2O 1 and [Co（4,4＇-bipy）2（H2O）4]DSNT·4,4＇-bipy 2 based upon the assembly of Co（II）, 4,4＇-bipyridine （4,4＇-bipy） and two new multifunctional organic ligands, 2,4,6-tris（4-sulfophenyl- amino）-1,3,5-triazine （H3TST） and 2,4-bis（p-sulfanilato）-6-diethylamino-1,3,5-triazine （H2DSNT）, have been prepared by hydrothermal method and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal structure of 1 is of monoclinic, space group P21/n with a = 13.599（4）, b = 18.988（6）, c = 22.995（7） A, β = 90.273（6）°, V = 5938（3）A^3, Z = 4, C56H59Co1.5N13O17S3, Mr = 1370.74, Dc = 1.533 g/cm^3, μ = 0.613 mm^-1, F（000） = 2842, GOOF = 1.018, the final R = 0.0796 and wR = 0.1498 for 9019 observed reflections with I 〉 2σ（I）. The crystal structure of 2 belongs to the monoclinic system, space group C2/c with a = 18.864（6）, b = 14.283（5）, c = 20.246（7）A, β = 107.799（6）°, V = 5194（3）A^3, Z = 4, C49H52CoN12O10S2, Mr = 1092.08, Dc = 1.397 g/cm^3, μ = 0.480 mm^-1, F（000） = 2276, GOOF = 1.059, the final R = 0.0665 and wR = 0.1900 for 4887 observed reflections with I 〉 2σ（I）. The results of X-ray crystal structure analysis revealed that complexes 1 and 2 exhibit layered supramolecular frameworks stabilized by electrostatic interactions, π-π interactions and hydrogen bonds.     

Synthesis and Crystal Structure of a Novel 3D Inorganic-organic Hybrid Metallic Coordination Polymer, [Na2Cd（2,6-pyda）（N3）2（H2O）6]n

A novel coordination polymer [Na2Cd（2,6-pyda）（N3）2（H2O）6]n （2,6-H2pyda = 2,6- pyridinedicarboxylic acid） has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c, with a = 24.416（4）, b = 10.7638（17）, c = 6.9224（11） A^°, β= 106.124（2）A^°, V = 1747.7（5） A^°3, Mr = 515.64, De= 1.960 g/cm^3,μ = 1.365 mm^-1, F（000） = 1024, Z = 4, the final R = 0.0426 and wR = 0.1320. In the title complex, there exist two kinds of metal centers in the structure, cadmium ions and sodium ions. The Cd（Ⅱ） atom shows a distorted pentagonal-dipyramidal geometry defined by two O and one N atoms from one deprotonated pyda ligand and four N atoms from four μ-1,1,3 azido groups. The adjacent cadmium atoms are bridged via two μ-1,1,3 azido groups, along the c axis to afford an extended chain. There is also a 2D network which is comprised of binuclear subunits [NaE（H2O）6] connected by O atoms from coordinated water between the adjacent Cdn（pyda）n（Na）2n infinite chains. Furthermore, each cadmium atom is connected with four adjacent sodium atoms through the bridging N3- ligand in μ-1,3 patterns. Thus, the title complex exhibits a novel three-dimensional network structure.     

Syntheses and Crystal Structures of Two New Compounds： [Zn（2,2＇-bipy）（L）Cl]2 and [Zn（phen）（L2）]2 （HL = 3-Methylbenzoic Acid）

Compounds [Zn（2,2＇-bipy）（L）Cl]2 1 and [Zn（phen）（L2）]2 2 （2,2＇-bipy = 2,2＇-bipyridine, HL = 3-methylbenzoic acid, phen = 1,10-phenanthroline） have been synthesized under hydrothermal conditions. 1： monoclinic, space group C2/c, a = 20.240（4）, b = 9.2960（19）, c = 17.904（4）A, β = 92.63（3）°, V = 3365.1（12） A^3, C36H30Cl2N4O4Zn2, Mr = 784.32, Z = 4, Dc = 1.548 g/cm^3, μ = 1.631 mm^-1, F（000） = 1600, the final R = 0.0367 and wR = 0.1289 for 3867 observed reflections （I 〉 2σ（I））. 2： monoclinic, space group C2/c, a = 23.035（5）, b = 9.0395（18）, c = 23.799（5） A, β = 98.55（3）°, V = 4900.6（17）A^3, C56H44N4O8Zn2, Mr = 1031.73, Z = 4, Dc = 1.398 g/cm^3, μ = 1.039 mm^-1, F（000） = 2128, the final R = 0.0540 and wR = 0.1287 for 5002 observed reflections （I 〉 2σ（I））. The two compounds have the same space group and similar isolated dinuclear structure, but different space packing structures are formed by different weak intermolecular interactions. Mo- reover, IR and luminescence spectra are also employed to study the crystal structures and pro- perties of these two compounds.     

Synthesis and Crystal Structure of a One-dimensional Silver（I） Coordination Polymer with 4,4＇-Bipyridine

The title compound, { [Ag2（bipy）2（H2O）2]·pydc·2H2O}n （bipy = 4,4＇-bipyridine, pydc = pyridine-3,5-dicarboxylate）, has been synthesized by the reaction of Ag2O with pydc and bipy in CH3OH solution. It crystallizes in the monoclinic system, space group C2/c with a = 21.419（8）, b = 7.515（3）, c = 18.070（7） A,β = 108.273（6）°, Mr = 765.27, V = 2761.9（17） A^3, Z = 4, Dc = 1.840 g/cm^3, F（000） = 1528,μ = 1.478 mm^-1, the final R = 0.0307 and wR = 0.0681. The structure determined demonstrated that the Ag（I） is three-coordinated by two nitrogen atoms from bipy and one water molecule, forming a one-dimensional coordination polymer [Ag2（bipy）2（H2O）2]n^2n＋, which is further linked to generate a two-dimensional layer structure via Ag---Ag attractions.     

Crystal Structure of Dimeric Units Cd2（ncpo）2（phen）2（H2O）2 Constructed by Flexible Dicarboxylic Acid with Fluorescent Emission

A dimeric coordination complex Cd2（ncpo）2（phen）2（H2O）2 was constructed by a flexible dicarboxylic acid, 2-nitro-4-carboxylphenoxyacetic acid. Its crystal structure was determined by X-ray single-crystal diffraction analysis. The crystal is of monoclinic system, space group P21/n with a = 17.2616（3）, b = 12.7460（2）, c = 18.4041（3） A^°, β= 94.432（1）°, C42H30Cd2N6O16, Mr = 1099.52, V = 4037.09（12）A^°^3 Dc = 1.809 g/cm^3, F（000） = 2192, μ = 1.139 cm^-1 and Z = 4. The final R = 0.0218 and wR = 0.0703 for 8288 observed reflections with I 〉 2σ（I）. There are two crystallographically independent but structurally very similar molecules in the unit cell of the title complex. It is noticeable that the ligand ncpo^2- displays a good flexibility, demonstrating different modes from the rigid ligands. The luminescence property has been investigated, which shows photoluminescence at 465, 490 and 574 nm upon excitation at 320 nm in the solid state at room temperature.     

Synthesis and Crystal Structure of a New Complex {[ Co^ⅢL2]·[Co^Ⅱ（H2O）6]0.6·2.25H2O }4 （H2L = N-（2-Hydroxyphenyl）salicylidenimine）

The reaction of Co（OAc）2·4H2O with the Schiff base H2L in a methanol solution affords the red crystals of { [Co^ⅢL2]·[Co^Ⅱ（H2O）6]0.5·2.25H2O}4 1 （H2L = N-（2-hydroxyphenyl） salicylidenimine）. The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n, C104Hi14Co6NaO37, Mr = 2421.61, a = 10.625（3）, b = 16.335（4）, c = 15.265（4）A^°, β = 102.990（4）°, V= 2581.6（11）A^°^3, Z = 1, Dc= 1.558 g/cm^3,μ = 1.034 mm^-1, F（000） = 1252, R = 0.0414 and wR = 0.1167 for 5889 reflections. The Co（HI） atom is six-coordinated by two nitrogen atoms and four oxygen atoms of two tridentate L ligands. The abundant hydrogen bonding interactions extend the complex into a one-dimensional supra- molecular framework. The uncoordinated water molecules act as space-fillers and consolidate the whole architecture through the hydrogen bonding interactions.     

Synthesis and Structure of a Hydrogen-bonding Assembled Three-dimensional Supramolecular Indium（Ⅲ） Compound Involving One-dimensional Helices

The title compound [In（H2ip）（pdc）（H2O）] （H3ip = 5-hydroxyisophthalic acid, H2Pdc = pyridine-2,6-dicarboxylic acid） has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 13.830（8）, b = 6.488（4）, c = 17.632（10）A^°, β = 92.510（10）°, C15H10InNO10, Mr= 479.06, V = 1580.6（15）A^°3, Z = 4, De= 2.013 g/cm^3, F（000） = 944,μ = 1.557 mm^-1, the final R = 0.0413 and wR = 0.0793 for 2950 observed reflections with I 〉 2σ（I）. The In（Ⅲ） ion is seven-coordinated in a slightly distorted penta-bipyramidal geometry. The mixed ligands connect the In（Ⅲ） ions into 21 helical chains along the [010] direction, and the hydrogen bonds assemble the chains into a three-dimensional supramolecular network.     

Crystal Structure and Inhibitory Activity against Xanthine Oxidase of Bis（μ2- chloro）-chloro-（μ-N,N＇-（2-pyridylmethylene） Furanmethanoamine Copper（II） Complex

A chloro-bridged dinuclear copper（H） complex with ligand 2-pyridylme-thylene- furfurylamine has been synthesized and characterized by single-crystal X-ray diffraction, and its inhibitory activity on xanthine oxidase （XO） was also evaluated. It crystallizes in the triclinic system, space group P 1 with a = 8.0441（16）, b = 8.5663（17）, c = 10.060（2）A, α = 77.52（3）, β = 72.04（3）, γ = 70.12（3）°, V = 615.3（2）A^3, Z = 1, Dc = 1.731 g/cm^3, F（000） = 322, the final R = 0.0401 and wR = 0.0934 for 1971 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the Cu（II） cation is five-coordinated by two N atoms of Schiff base and three Cl anions. The C-H…Cl intermolecular and intramolecular hydrogen bonds connect the molecules to form a three-dimensional network. This copper（II） complex shows more potent inhibitory activity against XO with IC50 = 3.48μM than the standard inhibitor allopurinol.     

A Facile Synthesis and Crystal Structure of 1-Amino-3-（2′-methylphenyl）isoquinolin Hydrochloride

The title compound （C16H15ClN2） has been synthesized by a facile self-condensation of o-tolunitrile promoted by potassium tert-butanolate in DMPU, and its structure was characterized by ^1H NMR, ^13C NMR, IR, UV, HRMS and X-ray single-crystal diffraction. The crystal belongs to orthorhombic, space group Pna21 with a = 19.560（3）, b = 7.8500（14）, c = 18.428（3） A^°, Dc = 1.271 g/cm^3, Z= 8, 2 = 0.71073 A^°,μ（MoKa） = 0.257 mm^-1, Mr = 270.75, V= 2829.5（8） A^°^3, Flack parameter = 0.12（12）, F（000） = 1136, the final R = 0.0571 and wR = 0.1445 for 2701 observed reflections with I 〉 20（I）. The intermolecular N-H…Cl hydrogen bonds link the molecules into a one-dimensional chain running along axis a.     

Hydrothermal Synthesis and Crystal Structure of a New Manganese（Ⅱ） Complex with 2,4-Pyridine-dicarboxylic Acid and 2,2′-Bipyridine Ligands

A new metal-organic complex [Mn2（PDC）2（bipy）2（H2O）2] （H2PDC = 2,4-pyridine-dicarboxylic acid, bipy = 2,2′-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The compound crystallizes in triclinic, space group P ^-1 with a = 7.376（3）, b = 9.990（4）, c = 11.950（5） A^°, α= 75.217（5）, β = 78.052（5）, γ = 70.655（5）°, V = 796.0（5）A^°3, C34HE6Mn2N6O10, Mr = 788.49, De = 1.645 g/cm^3,μ（MoKa） = 0.866 mm^-1, F（000） = 235, Z = 1, the final R = 0.0425 and wR = 0.0700 for 1971 observed reflections （I 〉 2σ（I））. In the crystal structure, the manganese atom is six-coordinated by two carboxylate oxygen atoms from two different PDC ligands, one aqua ligand, and three nitrogen atoms from 2,2′-bipy and PDC ligands, giving a distorted octahedral geometry. It exhibits a three-dimensional supramolecular network defined by O-H…O hydrogen-bonding interactions.     

Synthesis and Characterization of a Reduced Molybdenum（V） Phosphate,（H3dien）2（H2dien）2[NaMo12O24（OH）6-（H2PO4）（HPO4）5（PO4）2]·nH2O （n = 10.92）

A new reduced molybdenum（V） phosphate （H3dien）2（H2dien）2[NaMo12O24 （OH）6 （HEPO4）（HPO4）5（PO4）2]·nH2O （n= 10.92, dien = diethylenetriamine） has been synthesized under hydrothermal conditions and characterized by elemental analyses, IR and X-ray diffraction. C16H96.84MO12N12NaO72.92P8 （Mr = 3046.73） crystallizes in the monoclinic system, space group P21/c with a = 13.3575（18）, b = 21.907（3）, c = 15.654（2）A, β= 110.22（2）°, V= 4298.4（10） A^3 Dc = 2.354 g/cm^3, Z = 2,μ（MoKcr） = 1.966 mm^-1, F（000） = 2990.4, the final R = 0.0357 and wR = 0.1086 for 8739 observed reflections with I 〉 2σ（I）. It consists of sandwich-shaped cluster anions [Na{Mo6P4}2]^10- held together into a three-dimensional supramolecular framework through intermolecular hydrogen-bonding contacts. A probe reaction of the oxidation of acetaldehyde with H2O2 showed that this compound has high catalytic activity in the reaction.