Hydrothermal Synthesis and Structure of One New Vanadoarsenate [Zn（dien）（Hdien）]2[As6V15O42（H2O）]·4H2O

One new arsenic-vanadium cluster, [Zn（dien）（Hdien）]2[As6V15O42（H2O）]·4H2O （1, dien = diethylenetriamine）, has been hydrothermally synthesized and characterized by IR, elemental analysis, TGA, magnetic property and single-crystal X-ray diffraction analysis. Crystal data for 1： monoclinic, space group P21/n, a = 13.959（3）, b = 22.428（5）, c = 22.831（5） A^°, β = 90.733（4）°, Z = 4. X-ray crystallographic study showed that compound 1 is constructed from [As6V15O42（H2O）]^6- polyoxoanions linked together by novel [Zn（dien）（Hdien）]^3＋ complex fragments via hydrogen bonds into a three-dimensional network. Variable temperature susceptibility measurement demonstrates the presence of antiferromagnetic interaction between V^IV cations in 1.     

Synthesis and Characterization of a Bismuth Incorporating Heptamolybdate： （NH4）4 [HMo7O24Bi（H2O）2CsH3N（CO2）2]·7H2O

A new one-dimensional molecule based on the linkage of [Mo7024] clusters and [BiL] （L = pyridine-2,6-dicarboxylic acid） assembles under ambient conditions. The title compound was characterized by X-ray powder diffraction, IR and UV spectra, thermogravimetric analysis, and single-crystal X-ray diffraction. Crystal data： C7H38BiMo7N5037, Mr = 1664.95, monoclinic, space group C2/c, a = 24.312（2）, b = 21.4869（18）, c = 18.5423（16） A, β = 111.6490（10）°, V = 9002.9（13） A3, Z = 8, μ = 5.883 mm-1, F（000） = 6304, GOF = 1.045, R = 0.0365 and wR = 0.1062.     

Synthesis and Structure of a New Mixed-polyoxometalate （W/Mo） Compound： H5K{[Co（H2O）5]2（H2Mo3.24W8.76O42）}·19H2O

One new polyoxometalate compound connected via cobalt/potassium cations,namely H5K{[Co（H2O）5]2（H2Mo3.24W8.76O42）}·19H2O 1,was prepared and characterized by ele- mental analysis and IR spectroscopy. Single-crystal X-ray diffraction analysis result reveals that anions of {[Co（H2O）5]2（H2Mo3.24W8.76O42）}6- in compound 1 are linked by potassium cations to form one- dimensional chain,based on which a three-dimensional network is further constructed with the help of hydrogen bonds. Crystal data： H67Co2KMo3.24O72W8.76,Mr = 3297.87,monoclinic,C2/c,a = 19.0126（10）,b = 16.6025（5）,c = 19.1908（10）A,β = 106.713（1）°,V = 5801.8（5） A^3,Z = 4,Dc = 3.755 g/cm^3,F（000） = 5961,μ = 18.730 mm^-1,R = 0.0569 and wR = 0.1437 （I 〉 2σ（I））.     

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）.     

Synthesis,Crystal Structure and Characterization of a Cobalt Coordination Polymer： [Co（bib）（L）]-0.5H2O

The title coordination polymer, [Co（bib）（L）].0.5H2O 1 （bib = 1,1＇-（1,4-butanediyl）bis（imidazole） and L = 4,4＇-oxy（bisbenzoate） has been hydrothermally synthesized and characterized by IR and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group Cc with a = 8.8568（5）, b = 19.936（1）, c = 26.209（2） γ, y = 97.510（1）°, V= 4587.8（5） A3, Z = 8, CoC24H23N4O5.5, Mr = 514.39, Dc = 1.489 g/cm3, F（000） = 2128, μ（MoKa） = 0.795 mm^-1, R = 0.0419 and wR = 0.1002. Compound 1 exhibits a rare two-fold interpenetrating CdSO4 type topology. The O-H...O hydrogen bonds stabilize the structure of 1.     

Syntheses, Crystal Structures, and Properties of Two Mixed-ligand Coordination Polymers： [Zn（bdc）（1,3-bimb）]_n and {[Mn_2（ox）_2（1,3,5-tib）_（4/3）]·4H_2O}_n

Two new coordination polymers,[Zn（bdc）（1,3-bimb）]n（1） and {[Mn2（ox）2（1,3,5tib）4/3]·4H2O}n（2）（H2ox = oxalic acid,H2bdc = terephthalic acid,1,3-bimb = 1,3-bis（imidazol-1ylmethyl）benzene,1,3,5-tib = 1,3,5-tri（imidazol-1-yl）benzene）,were synthesized and characterized by elemental analysis,IR,powder X-ray diffraction（PXRD）,and thermogravimetric（TG） analyses.X-ray diffracation analysis reveals that two kinds of zigzag chains [Zn（bdc）]n and [Zn（1,3-bimb）]n in compound 1 are interweaved to form a 3D 4-fold interpenetrated 66-dia framework.In compound 2,Mn（1） and Mn（2） are linked via 1,3,5-tib ligands to form two different nets of [Mn6（1,3,5-tib）6 ]n along the ab plane with inner-or outer-shape N–Mn–N angles,which are connected by 1D infinite [Mn2（ox）2 ]n chains via Mn–O bonds to result in a（3,3,3,4,4）-connected（4·8·10）3（4·82）3（4·83·102）6（82·104·3）3（83）4 topology.Moreover,the photoluminescence of 1 has been investigated.The crystal of 1 crystallizes in orthorhombic,space group Pna2 with a = 13.2267（6）,b = 9.1717（4）,c = 17.4492（8）,V = 2116.79（16）3,Z = 4,C22 H18N4O4 Zn,Mr = 467.77,Dc = 1.468 g/cm3,F（000） = 960 and μ（MoKα） = 1.197 mm-1.The final R = 0.0280 and wR = 0.0618 for 3695 observed reflections with I 2（I） and R = 0.0389 and wR = 0.0653 for all data.The crystal of 2 crystallizes in rhombohedral,space group R-3 with a = 22.080（8）,c = 31.19（2）,V = 13167（11） 3,Z = 18,C24 H25 Mn2 N8 O13,Mr = 743.40,Dc = 1.688 g/cm3,F（000） = 6822 and μ（MoKα） = 0.945 mm-1.The final R = 0.0429 and wR = 0.1035 for 5160 observed reflections with I 2（I） and R = 0.0824 and wR = 0.1244 for all data.     

Synthesis,Crystal Structure and Antiproliferative Activity of 2-（（（5-（（（5,7-Dimethyl-[1,2,4]triazolo-[1,5-a]pyrimidin-2-yl）thio）methyl）-4-phenyl-4H-1,2,4-triazol-3-yl）thio）methyl）-4Hchromen-4-one Methanol Solvate

The novel crystal of the title compound 2-(((5-(((5,7-dimethyl-[1,2,4]triazolo-[1, 5-a]-pyrimidin-2-yl)thio)methyl)-4-phenyl-4H-1,2,4-triazol-3-yl)thio)methyl)-4H-chromen-4-one methanol solvate(C27H25N7O3S2, Mr = 559.66) has been prepared and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monocline system, space group P21/c with a = 11.9879(9), b = 14.0743(10), c = 15.9706(11), β = 98.509(2)°, V = 2664.9(3)3, Z = 4, Dc = 1.395 g/cm3, F(000) = 1168, μ = 0.116 mm-1, MoKa radiation(λ = 0.71073), R = 0.0652, and wR = 0.1425 for 5220 observed reflections with I 2σ(I). X-ray diffraction analyses reveal that the molecule adopts a C-shape. The planes of the benzopyrone and triazolopyrimidine were nearly parallel to each other, with a dihedral angle of 1.21(3)°. Intramolecular and intermolecular hydrogen bonds together with π-π interations are found to exist in the structure. The results of MTT assay indicate that the title compound displays excellent antiproliferative activity against two human cancer cell lines.     

A Novel Three-dimensional Extended Supramolecular Network Constructed from Octamolybdate Clusters and Morpholine Molecules： Nae（Hmorph）e[MosO26]·2H2O

A novel organic-inorganic hybrid, Na2(Hmorph)2[MosO26]·2H2O (1, Hmorph = morpholine), has been synthesized by convenient aqueous solution method and structurally characterized by single-crystal X-ray d...     

Synthesis and Structure of a POMs-based 3D Zeolike Ionic Crystal, {[Co（dpdo）2（H2O）2（CH3CN）]2（SiMo12O40）（H2O）2}n

A POMs-based 3D zeolike ionic crystal 1, {[Co（dpdo）2（CH3CN）（H2O）2]2（SiMo12O40）- （HEO）2}n （dpdo = 4,4＇-bipyridine-N,N＇-dioxide）, was constructed via self-assembly by embedding Keggintype [SiMo12O40]^4- polyanions within the intercrystalline voids as pillars and structurally characterized. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 11.430（3）, b = 12.242（3）, c = 14.279（3）A, α = 106.196（4）,β = 94.316（4）, γ = 98.294（3）°, V = 1884.5（7）A^3 Z = 1, C44H50N10O54CoEMo12Si, Mr = 2880.17, Dc = 2.538 g/cm^3, p = 2.484 mm^-1,F（000） = 1388, the final R = 0.0383 and wR = 0.1096 for 7753 observed reflections with I 〉 2σ（I）. Flack factor is 0.22（3）. Compound 1 is a pillar-layered framework with the [SiMo12O40]^4- anions linearly located on the square voids between the 2D bilayers which are formed by the dpdo ligands and cobalt（II） ions.     

Hydrothermal Synthesis and Crystal Structure of a Zinc（Ⅱ） Polymer with a Two-dimensional Layer Structure： [Zn（pzdc）（phen）]n·nH2O

A metal-organic coordination compound formulated as [Zn（pzdc）（phen）]n·nH2O 1 （H2pzdc = pyrazine-2,3-dicarboxylic acid, phen = 1,10-phenanthroline） has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a = 11.607（2）, b = 11.719（2）, c = 13.140（3）A^°, β = 110.707（3）°, V= 1671.9（6）A^°3, C18H12ZnN4O5, Mr= 429.69, De = 1.707 g/cm^3,μ（MoKa） = 1.511 mm^-1, F（000） = 872, Z = 4, the final R = 0.0356 and wR = 0.0853 for 2713 observed reflections （I 〉 2σ（I））. It exhibits an interesting two-dimensional layer structure and shows yellow photoluminescent property at room temperature.     

Synthesis,Structure, and Luminescent Property of a 3-D Zinc Complex { [ZN8II（4-APha）8（CH3COO）8] （CH3CH2OH）2}n①

The title complex [ZnⅡ8(4-APha)8(CH3COO)8(CH3CH2OH)2]n(1, 4-APha = 4-aminophenylhydroxamic acid) has been prepared under solvothermal conditions. It has been characterized by X-ray single-crystal diffraction, IR and elemental analysis. The crystal belongs to the monoclinic system, space group C2/c with a = 39.074(4), b = 9.9645(8), c = 38.846(3) A, β = 136.438 o, V = 10423.1(14) A3, C84H118N16O39Zn8, Mr = 2498.90, Z = 4, Dc = 1.592 g/cm3, μ = 1.900 mm-1, F(000) = 5144, the final R = 0.1036 and wR = 0.2953. This complex possesses a 3-D structure which is constructed from 1-D chain motifs linked by the 4-APha- ligands. The luminescent property of the title complex has been investigated.     

Synthesis and Crystal Structure of a Novel 2D Coordination Polymer [Cu_3（mal）_2（di-2-pyridlyktone）_2]

A novel coordination polymer of Cu II with flexible ligands,namely,[Cu 3 (mal) 2 (di2-pyridlyktone) 2 ] (1,H 2 mal=maleic acid),was synthesized and characterized by single-crystal X-ray diffraction,thermogravimetric analyses,elemental analysis and IR spectroscopy.The structure indicates that the complex crystallizes in monoclinic,space group P2 1 /c with a=10.268(2),b=17.737(3),c=8.038(1),β=98.275(2)°,V=1448.6(4) 3,Z=2,D c=1.883 Mg·m-3,μ=2.260 mm-1,F(000)=826,and the final R=0.0321 and wR=0.0820.In 1,three Cu II centers (Cu(1),Cu(2),Cu(1A)) are bridged by two uncommon μ 3-bridging H 2 mal ligands,furnishing a centrosymmetric trimetallic unit.Via further Cu-O COO coordination interactions,extention of these trimetallic units in two directions gives rise to an infinite corrugated 2D layer.In addition,thermal stability and electrochemistry of 1 were studied.     

A New 3D Supramolecular Network Formed by [Zn_3（2,6-Pyridinedicarboxylate）_3Cl_4]~（4-）and 4-Carboxypyridinium

A new compound [Zn3(C7NO4H3)3Cl4]·[C6NO2H6]4·4H2O (I) has been synthesized and structurally characterized by X-ray crystallography.It crystallizes in monoclinic,space group C2/c with a=16.9018(14),b=12.6902(10),c=25.1170(2),β=90.54°,V=5387.0(8)3,Z=4,Zn3C45H41Cl4N7O24,Mr=1401.76,Dc=1.728 g/cm3,F(000)=2840,μ(MoKa)=1.615 mm-1,the R= 0.0758 and wR=0.2060 for 3468 observed reflections (I 2σ(I)).Analysis of single-crystal X-ray diffraction data shows that compound I displays an interesting example of 3D supramolecular networks with perfect neutral and ionic hydrogen bonding array.     

Crystal Structure of a Novel Cadmium Coordination Polymer [Cd15（OH）4（SO4）4（L1）6（L2）12]n （HL1 = 1,2,3-1H-Triazole,HLe = 5-Methyl-lH-tetrazole

A novel cadmium coordination polymer [Cdls（OH）4（SO4）4（L1）6（L2）12]n （HL1 = 1,2,3-1H-triazole, HL2 = 5-methyl-lH-tetrazole） has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The compound crystallizes in cubicI-43d space group with a = 21.5247（4）, V = 9972.7（3） A3, Z = 4, Dc = 2.360 g/cm3, Mr = 3543.68, μ（MoKα） = 3.298 mm^-1, F（000） = 6696, the final R = 0.0340 and wR = 0.0992 for 1909 observed reflections （I 〉 2σ（I））. The compound contains two crystallographicatly independent Cd coordination centers linked up through one L1 and two L2 bridges. The structure displays an inorganic-organic hybrid cadmium coordination polymer.     

Synthesis,Structure Characterization and Photoluminescence of a Novel Complex with（6,4,4）-Network [Ce_2（2,5-pydc）_3（H_2O）_2]（2,5-pydc = Pyridine-2,5-dicarboxylic Acid）

A new three-dimensional supramolecular [Ce2(2,5-pydc)3(H2O)2](1) has been hydrothermally synthesized at 180 ℃ and characterized by single-crystal X-ray diffraction.X-ray crystal analyses reveal that the compound belongs to the monoclinic system,space group P21/c,C21H13Ce2N3O14,a = 6.561(1),b = 17.986(5),c = 9.411(3) ,β = 95.558(5)° and Z = 2.In the structure of 1,each Ce(1) center is surrounded by 2,5-pydc ligands,forming the 6-connected node,and the 2,5-pydc ligand coordinates to the Ce(Ⅲ) in two different coordination modes.In mode 1,the four oxygen atoms of two carboxyl groups connect neighboring Ce(Ⅲ) ions,giving 4-connected(4-c) second building unit(SBU-1).Furthermore,the structure is extended into a 2-D layer from SBU-1 by sharing Ce(1) atoms.In mode 2,the ligand coordinates to the Ce(Ⅲ) ion from the adjacent chain with the 4-connected(4-c) second building unit(SBU-2),generating a 1-D ladder from SBU-2 by sharing Ce(1) atoms.Finally,the structure is extended into a 6,4,4-c network.Its photoluminescence property was also investigated.     

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 Crystal Structure of N-[（2S）-4-bromo-2-（L-menthyloxy）-5-oxo-2,5-dihydro-3-furyl]-L-leucine

Starting from(5S)-(L-menthyloxy)-3,4-dibromo-5H-furan-2-one and L-leucine,the title compound N-[(2S)-4-bromo-2-(L-menthyloxy)-5-oxo-2,5-dihydro-3-furyl]-L-leucine 5(C20H32BrNO5,Mr = 446.37) was obtained in one-pot process via the tandem Michael addition-elimination reaction in the presence of potassium hydroxide.The chemical structure and absolute configuration of the title compound were confirmed via rotation,UV-Vis,FT-IR,1H NMR,13C NMR,MS and elemental analysis,especially by the X-ray single-crystal diffraction.The crystal crystallizes in an orthorhombic system,space group P212121 with a = 12.5249(16),b = 19.005(3),c = 19.719(3) ,V = 4693.7(10) 3,Z = 8,Dc = 1.263 g/m3,μ = 1.778 mm-1,F(000) = 1872,the final R = 0.0617 and wR = 0.1576 for 3967 observed reflections(I > 2σ(I)).X-ray analysis reveals that the title compound has two independent molecules in the asymmetric part of the unit cell with the two five-membered furanones being almost planar.The essential part of the electron delocalization is concentrated in the N(1),C(3),C(1),C(37) and O(7) region and N(2),C(28),C(27),C(30) and O(4) region in the other molecule respectively,but does not take place at the expense of delocalization within the ester function.     

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 New Dimolybdenum（V） Complex Na4[Mo2O4（HNTA）2]2·19H2O

The new binuclear molybdenum（V） complex Na4[Mo2O4（HNTA）2]2·19H2O （NTA = nitrilotriacetate） has been prepared and characterized by single-crystal X-ray diffraction analysis and IR. The crystal has space group Pnma with a = 10.2239（2）,b = 23.8174（3）,c = 23.1845（4） A,V = 5645.58（16）A^3,Z = 4,C24H66Mo4N4Na4O51,Mr = 1702.50,Dc = 1.958 g/cm^3,μ = 1.027 mm^-1,F（000） = 3280,T = 293（2） K,the final R = 0.0609 and wR = 0.1449 for 5512 observed reflections （I 〉 2σ（I））. Each MoV atom has a distorted octahedral coordination geometry,and the two coordination octahedra share a common edge to form a dioxo-bridged Mo2O4 unit which is coordinated by NTA ligands. The dianionic binuclear units [Mo2O4（HNTA）2]^2- are interconnected by Na^＋ into a layered structure.     

Synthesis, Structure and Dielectric Properties of a Novel 3D Gd（llI） Complex {[Gd（HPIDC）＇（μ4-C2O4）0.5＂H20]·2H2O}n

Under hydrothermal conditions, 2-（pyridin-4-yl）-lH-imidazole-4,5-dicarboxylaic acid （H3PIDC） reacted with Gd（NO3）3 to give a 3D complex {[Gd（HPIDC）＇a-C204）0.5＂H20]＂ 2H20}n （1）. Single-crystal X-ray determination shows that complex 1 crystallizes in the monoclinic system, space group P21/c with a = 8.287（8）, b = 14.796（14）, c = 11.559（11） ]k, fl = 90.969（15）, Z = 4, V = 1417（2） A3, C11H11GdN3Og, Dc = 2.280 g/cm3, Mr = 486.48, 2（MoKa） = 0.71073 A, p = 4.738 mm-1, F（000） = 936, R = 0.0248 and wR = 0.0522. Dielectric constant of complex 1 was measured at different frequencies with temperature variation.