Hydrothermal Synthesis, Crystal Structure and Fluorescent Property of a Novel Polyoxometalate [H6MoVI8O27]·3C4N2H10

A new infinite three-dimensional framework structure of the title compound [H6Mo^VI8O27]·3C4N2H10 has been synthesized under mild hydrothermal conditions and characterized by elemental analyses, IR, fluorescent spectra and single-crystal X-ray diffraction. C12H36Mo8N6O27 crystallizes in the triclinic system, space group P1^- with a = 8.820（3）, b = 9.534（3）, c = 10.993（4）A, α= 99.985（17）, β = 106.65（2）, γ= 101.650（14）°,V = 840.6（5）A^3, Mr = 1463.99, Z = 1, Dc = 2.892 g/cm^3,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 [H6Mo^VI8O27] subunit and three dissociated piperazine fragments. The complex exhibits two strong fluorescent emission bands at ca. 417 and 440 nm （λex = 378nm） in the solid state at room temperature.     

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.     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Novel Mo(V) Phosphate [Zn(Mo~v_6P_4O_(31)H_(10))_2(C_4H_(14)N_3)_2]·2C_4H_(13)N_3·8H_2O

1 INTRODUCTION Hydrothermal synthesis of Mo(V) phosphates has allowed various structures, all characterized by the presence of identical clusters with the composition Mo12MP8X62 (X = O, OH) to be stabilized[1～6]. Many Mo(V) phosphates with such clusters have been iso- lated to date. The first compound was discovered by Haushalter and Lai[1] for M = Na with the formula (PPh4)2[(H3O)2NaMo6P4O24(OH)7]?5H2O. Recently, a second type of structure has been observed for M = Na (Na8(…     

Hydrothermal Synthesis,Crystal Structure and Properties of a Novel Polyoxometalate {[Cu~Ⅱ(1,10-phen)]_2[PMo~Ⅵ_(11)Mo~ⅤO_(40)]} [Cu~Ⅰ(C_8N_4H_6)(C_9H_6NO)(H_2O)]

A new pseudo three-dimensional framework structure of the title compound {[CuⅡ(1,10-phen)]2[PMoⅥ11MoⅤO40]}[CuⅠ(C8N4H6)(C9H6NO)(H2O)](1) has been prepared by the hydrothermal method for the first time and characterized by elemental analyses,X-ray single-crystal diffraction and IR spectra.1 consists of two building blocks,one {[CuⅡ(1,10-phen)]2[PMoⅥ11MoⅤO40]} and one [CuⅠ(C8N4H6)(C9H6NO)(H2O)] coordinated group.Singlecrystal X-ray diffraction revealed that 1 crystallizes in the monoclinic system,space group P2/c with a=13.498(4),b=12.890(3),c=21.465(8),β=97.314o,V=3704(2)3,Mr=2693.61,Z=2,Dc=2.415 Mg/m3,μ=2.915 mm-1,F(000)=2562,S=1.009,the final R=0.0583 and wR=0.1406 for 5129 observed reflections with I2σ(I).Furthermore,compound 1 shows strong fluorescent properties in the solid state at room temperature.The electrochemical behavior of 1 has also been studied by cyclic voltammograms.     

Hydrothermal Synthesis and Crystal Structure of [H_4As_8V_(14)O_(42)(H_2O)]·6H_2O

1 INTRODUCTION The chemistry of polyoxometalates continues to attract interest as a result of their realized and potential applications in diverse fields, such as cata- lysis, analysis, biochemistry, medicine and material science[1～3]. In the past few …     

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,Structure and Magnetic Property of a Novel Hexa-Ni~Ⅱ Substituted Polyoxometalate

A novel hexa-NiⅡ substituted trilacunary Keggin polyoxometalate [{Ni6（μ3- OH）3（en）3（H2O）6}（B-α-PW9O34）]-6H2O 1 （en = ethylenediamine） has been hydrothermally synthesized and characterized by IR spectra, elemental analysis, thermogravimetric analysis （TGA）, single-crystal X-ray diffraction and magnetic property. Compound 1 crystallizes in the hexagonal space R3c with a = 20.4124（5）, c = 21.4427（4）A, γ = 120.000°, V = 7737.5（3）A3, Z = 6, GOF = 1.083, R （wR） = 0.0317 （0.0610）. Single-crystal X-ray diffraction indicates that 1 contains a hexa-Nin substituted trivacant Keggin [{Ni6（μ3-OH）3（en）3（H2O）6}（B-α-PW9O34）] unit. The magnetic study shows the presence of ferromagnetic coupling interactions within hexa-Nin clusters with J1 = 0.69 cm-1 and J2 = 0.92 cm^-1 for 1.     

Hydrothermal Synthesis, Crystal Structure and Fluorescence Property of a Novel Coordination Polymer [Eu_2(C_6H_8O_4)_3(H_2O)_2]_n·n(4,4′-bpy)

1UINTRODCTIONAtpresentthefluorescentmaterialsusedaremostlyinorganicororganicmicromolecularlumine-scentmaterialsthatareeasilyattenuatedinsunlight.Thereforepeopleintendtostudythepolymerflu-orescentmaterialscontainingrare-earthionsduetotheirgoodfluorescenthomochromepropertyandhighluminescentintensity.Inrecentyearswidestudieshavebeenperformed[1～10]tosearchforlu-minescentmaterialswithfineluminescentproper-tiesatlowprice.Asfortherare-earthcoordinationpolymer,agreatnumberofinvestigationsaremain…     

Synthesis and Crystal Structure of Compound 〔ZnS_6(C_(12)H_8N_2)〕

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Crystal Structure and Electrochemical,Fluorescent and Magnetic Properties of a New Complex [Ag(2,2ˊ-bipy)(C_(14)H_9O_3)]·(C_(14)H_(10)O_3)

A novel silver(I) complex [Ag(2,2ˊ-bipy)(C14H9O3)]·(C14H10O3) has been synthesized with 2-benzoylbenzoic acid as the ligand. Crystal data for the title complex: monoclinic, space group Cc, a = 27.4089(13), b = 10.2897(5), c = 12.0024(6)A, β = 111.864(4)o, Mr = 715.49, V = 3141.5(3) A3, Dc = 1.513 g/cm3, Z = 4, μ(Mo Kα) = 0.694 mm-1, F(000) = 1456, the final R = 0.0473 and w R = 0.1146. In the title complex, the central Ag(I) ion is located in a triangular coordination environment. The electron transfer is quasi-reversible in the electrode reaction and it shows a strong emission peak in the range of 495~520 nm under 502 nm excitation. In addition, it displays diamagnetic property from 3 to 300 K.     

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 and Crystal Structure of a Novel Supramolecular Compound [Mg(H_2O)_6](C_(16)H_(11)O_4SO_3)_2·10H_2O

IntroductionMolecularpolymerwithonedimensionalormultidimen sionalstructureassemblingthroughhydrogenbondsisanim portantresearchcontentinthesupramolecularchemistryandcrystalenginnering .1,2 Withthedevelopmentofnewtypefunctionalmaterialssuchasmolecularmagnetic ,selectedcatalysis ,reversiblecatalysis ,reversiblehost guestmolecular(ion)exchangeetc.,3themoleculardesignandsynthesishavealreadyattractedconsiderableattentioninsupramolecu larsystem .Thesupramolecularcomplexesandorganiccom poundscontainin…     

Synthesis and Crystal Structure of a 3-D Hydrogen-bonded Supramolecular Decavanadate Compound [Habo]_6[V_(10)O_(28)]·2C_3H_7OH·2H_2O

1 INTRODUCTION The chemistry of polyoxometalates has been at- tracting much attention due to the richness in their structures, electron and proton storage abilities, ther- mal stability and applications in catalysis, medicine and surface sciences[1～3]. In recent years, the mixed- valence as well as full oxidized vanadium polyoxo- anions have been crystallized with a variety of orga- nic molecules as counteranions[4～8]. However, the guiding principles of the crystal structures of poly- o…     

Syntheses and Crystal Structures of(H_3O)(C_3H_5N_2)[Mn(OH)_6Mo_6O_(18)]·3.5H_2O and (H_3O)_3[Co(OH)_6Mo_6O_(18)]·7H_2O

1 INTRODUCTION Polyoxometalates, a rich and remarkable classof inorganic cluster system[1], exhibit diverse appli-cation possibilities due to their topological and elec-tronic properties, ranging from their well-known roleas reagents in analytical, b…     

Syntheses and Crystal Structure of a New Molecular Clip Based on Diethoxycarbonyl Glycoluril: C_(54)H_(38)N_8O_6·H_2O

A new glycoluril derivative 2 has been synthesized and characterized by singlecrystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 13.128(7), b = 13.245(7), c = 14.016(8) ?, α = 98.805(10), β = 102.036(9), γ = 101.470(10)°, V = 2287(2) ?3, Z = 2, C54H38N8O6·H2O, Mr = 912.94, F(000) = 952, T = 298(2) K, Dc = 1.326 g/cm3 and μ = 0.090 mm-1. Due to the intermolecular C–H...O interactions, two monomeric molecular clips dimerize as a dimeric building block in the crystalline state. Those building blocks form tape-like supramolecular polymers driven by intermolecular C–H...N interactions and water molecules which stabilized in the packing structure served as hydrogen-bonding donors.     

Synthesis and Structure of a Novel Macrocyclic Ligand( C_(22) H_(29) N_3 O_3 Br_2)

１　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｍａｉｎｔａｒｇｅｔｉｎｍａｃｒｏｃｙｃｌｉｃｄｅｓｉｇｎｉｓｔｏｓｙｎｔｈｅｓｉｚｅｍａｃｒｏｃｙｃｌｅｓｗｈｉｃｈａｒｅａｂｌｅｔｏｄｉｓｃｒｉｍｉｎａｔｅａｍｏｎｇｔｈｅｄｉｆｆｅｒｅｎｔｍｅｔａｌｃａｔｉｏｎｓ．Ｍａｎｙｆａｃｔｏｒｓｉｎｆｌｕｅｎｃｉｎｇｔｈｅｓｅｌｅｃｔｉｖｉｔｉｅｓｏｆｍａｃｒｏｃｙｃｌｅｓｆｏｒｃａｔｉｏｎｓｈａｖｅｂｅｅｎｄｅｔｅｒｍｉｎｅｄｓｕｃｈａｓｓｕｂｓｔｉｔｕｅｎｔｅｆｆｅｃｔ，ｄｏｎｏｒａｔｏｍｉｃｔｙｐｅｓａｎｄ…     

Synthesis and Crystal Structure of Tetraacetyldiazidoacetyl-hexaazaisowurtzitane (C_(18)H_(22)N_(12)O_6·0.5CH_3COCH_3)

1　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｃｏｎｄｅｎｓａｔｉｏｎｏｆａｌｄｅｈｙｄｅｓｗｉｔｈａｍｉｎｅｓｉｓａｖａｌｕａｂｌｅｓｙｎｔｈｅｔｉｃｍｅｔｈｏｄｌｅａｄｉｎｇｔｏｐｏｌｙａｚａｐｏｌｙｃｙｃｌｉｃｓ,ｉｎｃｌｕｄｉｎｇｃａｇｅｄｃｏｍｐｏｕｎｄｓ.Ａｎｉｍｐｏｒｔａｎｔａｐｐｌｉｃａｔｉｏｎｏｆｔｈｉｓｒｅａｃｔｉｏｎｉｓｔｈｅｓｙｎｔｈｅｓｉｓｏｆｈｅｘａｂｅｎｚｙｌｈｅｘａａｚａｉｓｏｗｕｒｔｚｉｔａｎｅ(ＨＢＩＷ)ａｎｄｉｔｓｄｅｒｉｖａｔｉｖｅｓｗｉｔｈｓｕｂｓｔｉｔｕｔｅｄｂｅｎｚ…     

Synthesis and Crystal Structure of (C_6N_3H_(18))_2Ti_4O_4(C_2O_4)_7·4H_2O

1 INTRODUCTION The open-framework inorganic materials have been synthesized before the early 1980s[1]. Parti- cularly, metal phosphates have been investigated widely during the past few years[2, 3]. In recent years, considerable efforts have been devote…     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Cd(Ⅱ) Complex Based on Biimidazole and Isonicotinate-N-oxide

A new complex [Cd(H2biim)2(H2O)2]·(ino)2·4H2O (H2biim = 2,2'-biimidazole, ino = isonicotinate-N-oxide) has been prepared and characterized by single-crystal X-ray diffraction analysis, IR and fluorescence spectra analysis. The crystal is of triclinic system, space group P1 with a = 7.5380(6), b = 8.0402(7), c = 13.5094(11) , α = 104.269(1), β = 93.604(1), γ = 98.349(1)°, V = 780.93(11) 3, Mr = 765.00, Dc = 1.627 g/cm3, F(000) = 390, μ = 0.776 mm-1 and Z = 1. The final R = 0.0322 and wR = 0.0825 for 7038 observed reflections with I 2σ(I) and R = 0.0341 and wR = 0.0832 for all data. The title complex exhibits an infinite chain-like structure through bridging isonicotinate-N-oxide. Strong interchain hydrogen bonds between isonicotinate-N-oxide and H2biim result in the robust 3-D supramolecular architecture. Moreover, the complex shows strong photoluminescence with emission maximum at λ = 401 nm upon λex = 330 nm.     

Synthesis,Crystal Structure and Fluorescent and Thermal Stability Properties of the Zinc(Ⅱ) Complex [Zn(C_(15)H_(11)O_3)_2(C_(12)H_8N_2)_2]·5H_2O

A new complex has been synthesized with o-methylbenzoyl-benzoic acid(HL) and 1,10-phenanthroline(phen) in the mixture of water and ethanol. It crystallizes in monoclinic, space group C2/c with a = 13.6328(18), b = 17.7876(18), c = 19.998(2), β = 104.720(4)o, C54H48N4O11Zn, Mr = 994.33, V = 4690.2(9)3, Dc = 1.408 g/cm3, Z = 4, F(000) = 2072, μ(MoKα) = 0.59 mm-1, R = 0.0736 and wR = 0.2029. The crystal structure shows that the zinc ions are coordinated with two oxygen atoms from two HL molecules and four nitrogen atoms from two phen molecules, forming distorted octahedral coordination geometry. The fluorescent and thermal stability properties of the complex are studied. The result shows that it has one fluorescent emission band at around 412 nm. In addition, the complex is stable under 210 ℃.