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 (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) A, β= 110.22(2)°, V= 4298.4(10) (A)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.     

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 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[…     

Synthesis,Crystal Structure and Photoluminescence of [Gd(C_6NO_2H_5)_3-(H_2O)_2]_(2n)·(nH_5O_2)(nHgCl_5)(2nHgCl_4)·(2nH_2O)

A heterometallic 4f-5d inorganic-organic metal-isonicotinato hybrid Gd(C6NO2H5)3-(H2O)22n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O) 1 has been synthesized via hydrothermal reaction and structurally characterized.Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell:a=24.234(8)=b=20.816(7)=c=15.333(3)=β=128.091(8)°=V=6088(3)3=C36H47Cl13Gd2Hg3N6O20=Mr=2260.92=Dc=2.467 g/cm3=S=0.896=μ(MoKα)=10.331 mm-1=F(000)=4216=R=0.0344 and wR=0.0629.The crystal structure analysis reveals that the title complex is characteristic of a one-dimensional chain-like structure.Photoluminescent investigation reveals that the title complex displays a broad and intense emission in the green region.     

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 Crystal Structure Characterization of [Zr(HPO_4)(PO_4)F_2]·1.5H_3NCH_2CH_2NH_3

Thesynthesisofcrystallinezirconiumphosphateswasfirstreportedinl964byClearfieldandStynes['J,whodeterminedtheformulaasZr(HPO,),.H,O(a-ZrP)basedonchemicalcomposition,dehydrationandion-exchangebe-haviour'Sincethen,manyothercrystallinezirconiumphosphate,suchasZr(HPO,)(g-ZrP),Zr(HPO'),.H,O(Y-ZrP),havebeenprepared['.'1.Thesephosphatesconsistedofalternate,cross-linkedlayersofZrO,octahedraandPO'tetrahedrawithwatermoleculesaccommodatedininterlamellarfashion.a-Zirco-niumphosphate,Zr(HPO'),.…     

Hydrothermal Synthesis and Structure of a New Molybdenum Phosphate: (NH_3CH_2CH_2NH_3)_(2.5)[Mo_5O_(15)(PO_4) (HPO_4)]·7.5H_2O

1 INTRODUCTION A new class of materials of metal oxide clusters based on anionic molybdenum phosphate frameworks has received much attention as a consequence of their potential applications in catalysis and materials science [1]. As a result, some molybdenum phosphates have been studied [2,3]. Recently we have studied the structure of NaPMO material[4] and the spectrum of multicomponent compound with Keggin struc- ture [5]. Here we report the synthesis and crystal structure of a new…     

Synthesis,Crystal Structure,and Photoluminescent and Semiconductive Properties of [La(C_6NO_2H_5)_3-(H_2O)_2]_(2n)·(nH_5O_2)(nHgCl_5)(2nHgCl_4)·(2nH_2O)

A new heterometallic 4f-5d inorganic-organic metal-isonicotinic acid complex [La(C6NO2H5)3(H2O)2]2n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O) 1 has been synthesized via hydro-thermal reaction and structurally characterized. Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell:a =24.140(7),b=20.884(7),c=15.462(2),β=127.46(1)°,V=6187(3)3,C36H47Cl13Hg3La2N6O20,Mr=2224.24,Dc=2.388 g/cm3,Z=4,T=293(2) K,μ(MoKα)=9.401 mm-1,F(000)=4160 and R/wR=0.0376/0.0636 for 4130 observed reflections (I > 2σ(I)) and 5617 unique reflections. Complex 1 is characteristic of a one-dimensional polycationic chain-like structure. Photoluminescent investigation reveals that the title complex displays interesting emissions in violet and orange regions. The luminescence spectra show stronger orange emission than violet emission. Optical absorption spectra of 1 reveal the presence of a wide optical bandgap of 3.41 eV.     

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.     

新型杂多蓝化合物[NH_3(CH_2)_2NH_3]_5[Cd(H_2O)][CdMo_(12)~ⅤO_(30)(HPO_4)_6(H_2PO_4)_2]·5H_2O的合成与晶体结构

利用水热法首次合成了具有两种配位环境Cd原子的新型杂多蓝化合物[NH3(CH2)2NH3]5[Cd(H2O)][CdMo12ⅤO30(HPO4)6(H2PO4)2].5H2O.通过元素分析I、CP、TG和X射线单晶衍射确定了其组成,使用IR和EPR进行了结构表征.通过N2吸附脱附测定了比表面积和孔径,为催化研究提供了基础数据.结果表明:该晶体为三斜晶系,P-1空间群;晶胞参数a=1.200 2(2)nm,b=1.465 1(3)nm,c=2.119 2(4)nm,V=3.564 2(12)nm3,β=83.01(3)°,Z=2,F(000)=293 2,R1=0.030 0,wR2=0.071 6.     

A Novel 3D Extended Network Cobalt Paradodecatungstate:Synthesis,Characterization and Crystal Structure of [Co(H_2O)_5]_2[Co(H_2O)_4]_3[H_2W_(12)O_(42)]·11H_2O

1 INTRODUCTION Polyoxometalates are the unique metal-oxygen clusters composed of transition metals in groups V and VI (Mo, W, V, Nb, Ta) in a high oxidation state showing a large structural varieties as well as inte- resting physical and chemical properties in diverse fields including catalysis, analytical chemistry, nanotechnology, chemical sensing, biochemical and geochemical processes, medicine and materials science[1～5]. Recently, there has been increasing interest in the synthesis…     

Non-Isothermal Decomposion Kinetics of Supermolecule Compound [Eu(C_(10)H_9N_2O_4)(C_(10)H_8N_2O_4)(H_2O)_3]_2·phen·4H_2O

Europium(Ⅲ) compound with 2-oxopropionic acid salicyloyl hydrazone (C_(10)H_(10)N_2O_4,H_3L) and 1,10-phenan-throline (C_(12)H_8N_2,phen) has been prepared.A yellow prismatic crystal of the compound was obtained,and themolecule crystallized in the triclinic space group P-1.There are two 9-coordinated complex molecules in everystructure unit,where every Eu atom is coordinated by three water molecules and two tridentate C_(10)H_(10)N_2O_4 ligands,forming two stable pentacycles.The coordination polyhedron around Eu~(3+) was described as a single cap squareantiprism.In the crystal cell,there are one free 1,10-phenanthroline and four water molecules.The thermaldecomposition of the compound and its kinetics were studied by non-isothermal thermogravimetry.The Kissinger'smethod and Ozawa's method were used to calculate the activation energy value of the first-step decomposition.Thestages of the decompositions were identified by TG-DTG-DSC curve.The non-isothermal kinetic data were ana-lyzed by means of integral and differential methods.The possible reaction mechanism and the kinetic equationswere investigated by comparing the kinetic parameters.     

K_4Na_2{Cu[C(CH_3)(OH)(PO_3)_2]_2}·12H_2O络合物的晶体结构研究

K_4Na_2{Cu[C(CH_3)(OH)(PO_3)_2]_2}·_(12)H_2O络合物晶体属三斜晶系,空间群为C~1_i-P;a=11.951(3),b=6。220(1),c=11.789(2)A;a=113.166(11)°,β=108.944(15)°,γ=97.563(14)°;V=727.4A~3;D_c=2.02g/cm~3;μ_(MoKa)=16.9cm~(-1)。结构分析证实Cu~( 2)与2个HEDP配体形成了六啮六环的螫合离子,6个Cu—O配住键包含有键距为2.667A2个长键。R=0.0413。     

三价铬丙二酸配合物[Cr(C_3H_2O_4)(H_2O)_4][Cr(C_3H_2O_4)_2(H_2O)_2]·4H_2O的合成、晶体结构及性质研究

在三重桥氧三核铬羧酸配合物的系列研究中,采用与铬的一元羧酸配合物类似的实验条件,以丙二酸为配体合成了不同构型的配合物[Cr(C_3H_2O_4)(H_2O)_4)][Cr(C_3H_2O_4)_2(H_2O)_2]·4H_2O,通过X射线衍射测定了其单晶结构,并对-COO的配位方式作了讨论,还研究了配合物的红外光谱、拉曼光谱、紫外可见光谱、质谱、磁化率等性质,探讨了性质与结构的关系,并由此论证了二元羧酸和铬形成的双齿螯合构型化合物的稳定性.     

Synthesis and Structure of(NH4)_2 [V2O_4(OCH_2COO)_2]

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆ（ＮＨ４）２［Ｖ２Ｏ４（ＯＣＨ２ＣＯＯ）２］ＺＨＯＵＺｈａｏ－ｈｕｉ，ＷＡＮＧＪｉｎｚｈｉ，ＷＡＮＨｕｉ－ｌｉｎａｎｄＴＳＡｌＫｈｉ－ｒｕｉ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ，ＸｉａｍｅｎＵｎｉ...     

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 …     

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 Crystal Structure of [Zn(HPDB)_2(H_2O)_2]n·2nDMSO·2nH_2O (H_2-PDB = Pyridine-3,4-dicarboxylic Acid)

1 INTRODUCTION Metal-organic coordination polymers are currently of considerable interest and importance because they can be used as new functional materials applicable in adsorption, luminescent and NLO materials fields[1, 2]. Due to the manifold N- and O-donors of pyridine- (bi)carboxylic ligands, metal pyridine-(bi)carboxyla- tes can construct versatile structural motifs, which finally aggregate to generate various supramolecular architectures with interesting properties[3, 4]. The d…     

Synthesis and Characterization of a One-dimensional Chain Polymer{[Cu(4-CPOA)(3-PyOH)_2(H_2O)_2]·H_2O}_n

1 INTRODUCTION Molecular self-assembly of coordination architec- tures is a rapidly developing research area of supra- molecular chemistry in recent years[1～6]. 4-Carboxy- phenoxyacetic acid (4-CPOAH2) is a multidentate flexible and rigid ligand, which is capable of coor- dinating to metal centers in versatile binding fashi- ons and can also form regular hydrogen bonds as both hydrogen-bond donors and acceptors. To date, only Na(I), Ni(II), Mn(II) and Co(II) complexes con- taining…     

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.