Hydrothermal Synthesis and Characterization of a Novel Two-dimensional Framework Materials Constructed from Polyoxometalate and Coordination Groups:[H2Mo5.5V10.5O40(PO4)][Cu(en)2]4·7H2O

A novel compound [H2Mo5.5V10.5O40(PO4)][Cu(en)2]4*7H2O(1) was synthesized from V2O5, MoO3, CuCl2*2H2O, en, H3PO4 and H2O in an aqueous solution via the hydrothermal method and characterized by means of single-crystal X-ray diffraction, elemental analyses, IR, EPR spectra and thermal analyses. C16H80Cu4Mo5.5N16O51PV10.5 crystallized in a triclinic system, the space group is P1 with M=2660.63, a=1.283590(10) nm, b=1.289910(10) nm, c=1.387870(10) nm, V=1.80942(2) nm3, Z=2, Dx=4.883 g/cm3, F(000)=2599, μ=6.956 mm-1, (Δ/σ)=0.000, S=1.089. The crystal structure was solved by the direct methods with the final R=0.0752 and wR=0.1988 for 6311 observed reflections with I≥2σ(I). The X-ray crystallography reveals that compound 1 is a novel two-dimensional framework material constructed from the mixed Mo/V polyoxometalate and coordination groups.     

Hydrothermal Synthesis and Characterization of [V_(16)O_(38)(Cl)][Cu(enMe)_2]_(3.5)·2H_2O Containing {V_(16)O_(38)} Cluster

IntroductionBasedonarelativelylargenumberofdifferenttypesofbuildingblockswhichcorrespondtopolyhe dron {VOx} (x =4 ,5 ,6 ) ,polyoxovanadatesshowanextraordinaryvarietyofstructures ,suchascage ,basket ,belt ,ballandbarrelstructures[1— 5] .Further more,these polyoxovanadatesexhibita pronouncedtendencytoformcage likestructureswhichmayen capsulateneutralmoleculesaswellasionicguests ,afeaturesharedbysomeisopolyanionssuchas [V18O4 2·(H2 O) ]12 - [6 ] ,[H4 V18O4 2 (X) ]9- (X =Cl- ,Br- ,I- ) [2 ,…     

Hydrothermal Synthesis and Crystal Structure of Iron Molybdophosphate Fe[Mo_6O_(12)(OH)_3(H_2PO_4)(HPO_4)_2(PO_4)]_2- [Fe(2,2′-bipy)(H_2O)_2]_2[Fe(2,2′-bipy)_3]_2·6H_2O

1 INTRODUCTION Organic-inorganic hybrid materials and polyoxo-metalates have received much attention because of their intriguing structural diversity and potential applications in molecular adsorption, ion exchange, heterogeneous catalysis and nanotech nology as well as in electrical, magnetic and photochemical areas[1, 2]. One of the important ad- vances in the design of new organic-inorganic hybrid materials is utilizing poly- oxometalates’ coordination ability to produce poly- oxoanio…     

Hydrothermal Synthesis and Structure of a Novel Two-dimensional Complex:[Ni_(0.5)(H_2O)_(1.5){Ni(en)_2}_3V_(18)O_(42)(Cl)]3.5H_2O

1 INTRODUCTION The crystal engineering of inorganic-organic hybrid materials has generated significant interest in their new structural architectures and potential ap- plications in the fields of photochemistry, catalysis, electromagnetism and sorption[1…     

A Pseudo-Keggin Compound: Hydrothermal Synthesis and Crystal Structure of (DETAH)(DETAH_3)_3[V_(18)O_(42)(PO_4)]·(PO_4)·2H_2O

The novel vanadophosphate (DETAH)(DETAH3)3[V18O42(PO4)]·(PO4)·2H2O has been synthesized under hydrothermal conditions and its structure was determined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic, space group C2/c with a = 23.857(3), b = 12.9619(18), c = 20.204(3) , β = 105.692(2)°, V = 6015.0(14) 3, Z = 4, Dc = 2.473 g/cm3, Mr = 2239.68, F(000) = 4432, R = 0.0725, wR = 0.1524 and GOOF = 1.095. The metaloxo cluster contains a novel six-capped pesudo-Keggin structure unit which encloses a disorder PO43- guest.     

Hydrothermal Synthesis and Structure of a Novel Molybdenum Phosphate: Na_4(H_3O) [Na(HPO_4)_2(PO_4)_4Mo_(18)O_(49)]·16H_2O

1 INTRODUCTION The design synthesis of metal oxide heterpoly compounds have been the subject due to their diverse structures and potential applications in catalysis, sorption, electrical conductivity, ion exchange and anti-virus[1]. Molybdenum phosphates with microporous framework serve as a new kind of inorganic microporous materials. In the course of our investigation on the synthesis of Molybdenum phosphates, we have hydrothermally synthesized an organically templated solid material[…     

Hydrothermal Synthesis and Crystal Structure of a Novel Polyoxometalate K(C_4N_2H_(12))_4(C_4N_2H_(11))_(2-)[Mo_8~ⅤMo_4~ⅥCdP_8O_(54)(OH)_8]F·6H_2O

The title compound 1 has been synthesized by the reaction of H_2MoO_4, CdCl_2, H_3PO_4, KF, piperazine hexahydrate and water in aqueous solution under mild hydrothermal conditions. Single-crystal X-ray analysis reveals that the title compound crystallizes in the triclinic system, space group P(-1) with a = 14.049(3), b = 15.972(3), c = 20.043(4) (A), α = 85.82(3), β = 81.28(3),γ = 67.15(3)°, V= 4095.9(14) (A)~3, M_r = 3204.62, Z=2,D_c = 2.598 g/cm~3,μ = 2.360 mm~(-1), F(000) = 3124, the final R = 0.0314, wR = 0.0826 and S = 0.989 for 18592 observed reflections with I > 2σ(I). The crystal packing is stabilized by N-H…O and O-H…O intra- and intermolecular hydrogen bonds to form an infinite 3D network.     

Synthesis, Structure Characterization and Biological Activity of a Novel Polyoxovanadate Cluster: [NH_3(CH_2)_2NH_2(CH_2)_2NH_3]_4·[V_6~Ⅴ V_(12)~Ⅳ O_(42)(PO_4)](PO_4)·2H_2O

IntroductionPolyoxometalates(POMs)have been attracting ex-tensive interest in solid state material chemistry due tothe richness of their structures and special properties incatalysis,photochemistry,electro-chromism and mag-netism[1—3].POMs have also attracted increasing inter-est of biochemists because of their potential applicationsas drugs againsttumors and viruses[4—6].Agood way todesign drugs based on POMs is to modify the polyox-oanion frameworks with appropriate chemicals,such asami…     

Synthesis and Characterization of a Reduced Molybdenum(V) Phosphate, (H_3dien)_2(H_2dien)_2[NaMo_(12)O_(24)(OH)_6-(H_2PO_4)(HPO_4)_5(PO_4)_2]·nH_2O (n = 10.92)

A new reduced molybdenum(V) phosphate (H3dien)2(H2dien)2[NaMo12O24 (OH)6 (H2PO4)(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) , β = 110.22(2)°, V = 4298.4(10) 3, Dc = 2.354 g/cm3, Z = 2, μ(MoKα) = 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.     

Synthesis and Structural Characterization of a Novel Coordination Polymer [Cd(C_4H_2O_4)(C_3H_4N_2)_3]_n·2nH_2O

1 INTRODUCTION In recent years, the design and synthesis of metalorganic coordination polymers have attracted considerable attention, for such supramolecular assemblies have interesting structures as well as potentiaapplications as smart optoelectronic, magnetic andporous materials. By judicious selection of ligandand metal coordination geometries, control over thetopology and geometry of the infinite networks canbe gained. As neutral donor ligands, 4,4?-bpy, pyrazine and imidazole which …     

Synthesis and Structural Characterization of a Novel Sphere Compound of Mo_8V_2O_(28)·7H_2O

Polyoxometalates( POMs) are attractivebuilding blocks for functional materials withpotential application in electrocatalysis and thepreparations of molecular electronic,orelectrooptical devices[1,2 ] . With the recentdiscovery of giant nanoporous and spherePOMs[3— 6] ,it remains a great challenge tosynthesize rationally new nanoscale materialspossessing novel structures and desirableproperties.The present paper covers a novelstructure characterization of Mo8V2 O2 8· 7H2 O( abbreviated Mo…     

The Synthesis and Structural Characterization of Two-dimensional Coordination Polymer {[Ni(phen)H_2O](μ_4-C_( 10)H_2O_8)_(1/2)}_n

The successful preparation of coordinationpolymers from modular precursors has provided afacile approach to develope solids and functionalmaterials[1— 4 ] . A popular strategy that could beemployed in the area is the adoption of bridgingligands such as cyanide,bi- pyridine,benzenetricarboxylate,etc.[3— 8] . In this context,multi- connecting carboxylates are at presentespecially interesting because they exhibit richcoordination chemistry by coordinating to metalions and have been proved to be…     

Hydrothermal Synthesis and Structural Characterization of a Novel 3-D Open Framework Zinc Phosphate Microporous Compound(C_5N_2H_(14))·[Zn_3(OH_2)(PO_4)_2(HPO_4)]

One novel organically templated zincophophate(C5N2H14)·[Zn3(OH2)(PO4)2(HPO4)] has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction together with elemental analysis, infrared spectroscopy, thermogravimetric analysis, and powder X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/n, with a = 9.7904(11), b = 14.0287(14), c = 11.8651(13) , β = 104.690(3), V = 1576.4(3) 3, Z = 4, T = 296(2) K, Mr = 601.31 and Dc = 2.533 g/cm3. The compound consists of a macroanionic [Zn3(OH2)(PO4)2(HPO4)]2- framework and(C5N2H14)2+ cations, and its structure is built up from ZnO3(OH2), ZnO4, HPO4 and PO4 tetrahedral units that result in 4, 8 and 10-ring channels.     

Synthesis and Structural Characterization of {[Mn(phen)_2(OAc)(H_2O)]ClO_4}_2H_2O

1 INTRODUCTION Chemistry of manganese cluster has become an attractive research field because of the involvement of manganese in several biological redox-active sys- tems[1,2], especially in the oxygen-evolving complex (OEC) of photosystem Ⅱ (PSⅡ) in green plants[3]. It was thought that the coordination environment of Mn in OEC contains O and N donors, and the bind- ing of aqua to the Mn site may be important to the oxidation of aqua for the evolution of dioxygen[4, 5]. In recent …     

Hydrothermal Synthesis, Structural Characterization and Properties of Mixed Valent Decavanadium Oxide [Co_2Cl_8V_(10) O_(18)(H_2O)]Cl_2·6H_2O with Novel Three-dimensional Framework

IntroductionPolyoxometalates constitute an enormous classof compounds whose unusual versatility and reac-tivity afford practical applications to many fields,such as catalysis,biology,medicine,and materialsciences[1— 4] .In recent years,hydrothermal tech-nique has become a vital tool in self- assemblychemistry.This technique,in combination with or-ganic templates,has been demonstrated to be wellsuited for the synthesis and the crystal growth ofpolyoxometalates with novel structures[5— 9] .Amo…     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Coordination Polymer Constructed from Bicapped Pseudo-Keggin Cluster:(Et_3N)_(0.5)(en)_2[SiMo_(12)O_(40)(VO)_2]·4H_2O

A new pseudo Keggin-type bicapped compound(Et3N)0.5(en)2[SiMo12O40(VO)2]·4H2O(Et3N=triethylamine,en=ethylenediamine) has been hydrothermally synthesized and characterized by IR,elemental analysis,TG and X-ray crystallography.The title compound crystallizes in monoclinic,space group P21/n with a=17.576(2),b=13.535(1),c=21.587(2),β=103.790(10)°,V=4987.3(8)3,Z=4,Dc=2.925 Mg/m3,Mr=2196.12,F(000)=4148,μ=3.400 mm-1,R=0.0379 and wR=0.1219.The most remarkable structural feature of the compound is that the clusters represent bicapped pseudo-Keggin structure and are linked one by one through V-O-V bonds forming an infinite 1D chain.Furthermore,such chains are interconnected in a cross-like arrangement through multiform hydrogen bonds to yield a 3D supramolecular network.     

Mo_8~ⅤW_2~ⅥO_(26)(C_5H_5N)_8·2H_2O: A Novel Mixed-valence Heterometal Polyoxometalate

A new mixed-valence heterometal cluster Mo8VW2VIO26(C5H5N)8·2H2O has been synthesized under solvothermal conditions and characterized by X-ray single-crystal diffraction, IR, UV-vis and XPS spectroscopy. The title compound crystallizes in the triclinic system, space group P1 with a = 11.708(3), b = 12.018(4), c = 13.316(4) , a = 112.184(4), β = 97.844(4), r = 110.043(3)o, V = 1551.9(8) 3 and Z = 1 at 293(2) K. The final full-matrix least-squares refinement converged to R = 0.0414 for 4460 observed unique reflections with I 2σ(I) and w R = 0.1290 for all data(5352) and S = 1.015. In addition, its thermal stability and fluorescent property have also been investigated.     

Synthesis,Structure and Polymorphism of a Novel Two-dimensional Cobalt(Ⅱ) Coordination Polymer Constructed from Citrazinate Ligand

The polymeric Co(Ⅱ) complex[Co(Hdhpc)(py)]_n(1)(py = pyridine,H_3dhpc =2,6-dihydroxypyridine-4-carboxyl acid) was prepared and characterized.X-ray diffraction data revealed that the compound crystallizes in dimorphic 1α and 1β forms at room and low temperature,respectively.The former crystallizes in the orthorhombic crystal system,space group Pbcm with a =7.209(1),b = 14.834(3),c = 15.376(3) ?,V= 1644.3(5) ?~3,Z = 4,C_(16)H_(13)CoN_3O_4,M_r = 370.22,D_c= 1.496 g/cm~3,F(000) = 756,μ = 1.068 mm~(-1),R = 0.0633 and wR = 0.1192.While 1β is attributed to the monoclinic space group C2/c with a = 32.102(4),b = 7.022,c = 14.945(2) ?,β = 109.052(5)°,V= 3184.4(6) ?~3,Z= 8,D_c= 1.544 g/cm~3,F(000) = 1512,μ = 1.103 mm~(-1),R = 0.0428 and wR =0.0797.The conformation changes of pyridines between Co-citrazinate planes leading to a reversible single-crystal to single-crystal transformation.The variable temperature magnetic data indicate a weak ferrimagnetism.     

A Novel Layered Complex with Rhomboidal Channels:Hydrothermal Synthesis,Crystal Structure,and Properties of Cu(4,4''''-bipy)_2(H_2PO_4)_2(H_2O)_2 (bipy=bipyridine)

IntroductionMetalcoordinationpolymerswithvariablechan nelsorcavitiesarecurrentlyofinterestduetotheirpotentialfunctionsasmicroporoussolidmaterialsformolecularadsorption ,ionexchange ,molecularmag nets,andshape selectivecatalysis[1— 3] .Amajorre searchefforthasbeenfocusedonusingthemolecularbuildingblockapproachtogeneratesuchmicroporousmaterials[3— 5] .Beinganalogoustopyrazine ,therigidrod like 4 ,4′ bipyridine(4 ,4′ bipy)ligandisausefulbuildingblockfortheconstructionofmetal organicco ordinat…     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Novel Polyoxometalate [H_6Mo_8~(VI)O_(27)]·3C_4N_2H_(10)

A new infinite three-dimensional framework structure of the title compound [H6MoVI8O27]·3C4N2H10 has been synthesized under mild hydrothermal conditions and charac-terized by elemental analyses,IR,fluorescent spectra and single-crystal X-ray diffraction.C12H36Mo8N6O27 crystallizes in the triclinic system,space group P 1 with a = 8.820(3),b = 9.534(3),c = 10.993(4) ,α = 99.985(17),β = 106.65(2),γ = 101.650(14)o,V = 840.6(5) 3,Mr = 1463.99,Z = 1,Dc = 2.892 g/cm3,μ = 2.993 mm-1,F(000) = 702,the final R = 0.0676,wR = 0.1920 and S = 1.074 for 2196 observed reflections with I > 2σ(I).The title compound exhibits a novel infinite three-dimensional(3D) framework composed of a [H6MoVI8O27] subunit and three dissociated piperazine fragments.The complex exhibits two strong fluorescent emission bands at ca.417 and 440 nm(λex = 378 nm) in the solid state at room temperature.