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'),.…     

Synthesis, Structure Characterization and Biological Activity of a Novel Polyoxovanadate Cluster: [NH3(CH2)2NH2(CH2)2NH3]4·[VⅤ6VⅣ12O42(PO4)](PO4)·2H2O

A new polyoxovanadate cluster,[NH3(CH2)2NH2(CH2)2NH3]4[VⅤ6VⅣ12O42(PO4)](PO4)·2H2O, has been synthesized and characterized by means of elemental analysis, IR spectrometry, EPR spectrometry, TG analysis and single crystal X-ray diffraction. This compound crystallizes in a monoclinic space group C2/c with a=2.3912(5) nm, b=1.3002(3) nm, c=2.0172(4) nm, β=105.75(3)°, V=6.036(2) nm3, Z=2, R1=0.0572, wR2=0.1476. It has a superKeggin structure with a Keggin unit capped by six [VO5] moieties on the pits on every side of the Keggin unit. The anti-tumor activity of the compound was estimated in three human tumor cell lines in vitro.     

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.     

(NH_2CH_2CH_2NH_3)_4[W~ⅤO_2(OC_6H_4O)_2]_2(NH_3CH_2CH_2NH_3)·H_2O的合成、晶体结构、EPR以及与同构物的比较

在很多生物代谢过程中,微量元素W起着关键作用,W与生物大分子结合形成具有特异功能的钨氧转移酶。1983年从热醋酸菌中提取了第一种钨酶,即甲酸脱氢酶,目前从生物体内提取的钨酶种类已达十二种之多,并发现钨氧转移酶与钼氧转移酶的活性结构因子呈相近性[1]。随着钨酶在生物体内的作用逐步得到重视,及其模拟的功能配合物在探究钨酶的生理活性和催化机理研究中所作的突出贡献,使钨氧转移酶活性结构因子的仿生合成、生理活性以及催化机理研究成为研究热点[2￣14]。根据报道显示,单分子的钨氧模拟配合物中W的价态只有WⅣ、WⅥ两种,且形成一个电…     

Hydrothermal Syntheses, Crystal Structure and Thermal Behavior of [(CH_3)_2NH_2]_2[B_5O_6(OH)_4]_2·[HCON(CH_3)_2] and [NH_3CH_2CH_2NH_3]_2·[B_(14)O_(20)(OH)_6]

Two novel organic base templated nonmetal borates [(CH₃)₂NH₂]₂[B₅O₆(OH)₄]₂·[HCON(CH₃)₂] ( ? ) and [NH₃CH₂CH₂NH₃]₂[B₁₄O₂₀(OH)₆] ( II ) have been synthesized under hydrothermal conditions, and characterized by elemental analyses, FT‐IR spectroscopy, X‐ray diffraction, and TG‐DTA. Their crystal structures were determined from single crystal X‐ray diffraction. The crystal structure of compound I is characterized by forming a 3D supramolecular structure with large channels along axes b and c through O? H···O hydrogen‐bonding among the [B₅O₆(OH)₄]^? anions. The crystal structure of compound II is characterized by forming a 3D supramolecular structure with large channels along axis a and direction [111] through O? H···O hydrogen‐bonding among the [B₁₄O₂₀(OH)₆]^4? anions. The templating organic amine cations in I and II are both obtained through in situ hydrothermal reactions, and are both located in the channels of the 3D supramolecular structure, respectively. Their thermal behavior has been also investigated.     

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.     

一种二帽pseudo-Keggin结构簇合物[HN(C_2H_5)_3]_3[N(C_2H_5)_3]_2[Mo_8~ⅣMo_4~ⅤV_2~ⅣO_(38)(PO_4)]的水热合成、结构和性质研究

金属－氧簇合物因其结构多样性及在催化、材料和医药等方面的应用而引起人们的关注犤１犦。在众多金属－氧簇合物中，Keggin结构及金属取代Keggin结构金属－氧簇被大量报道，但由于很难获得高质量单晶，有关二帽Keggin结构的报道非常少，目前只有几例报道犤２～９犦。近年来，随着水热法应用到金属－氧簇的合成，陆续获得了一系列具有新颖结构的簇合物。１９９８年，通过水热法获得了第一个二帽pseudo－Keggin结构簇合物犤NH４犦４H犤PMo８VⅣ４VⅤ２O４２犦·２４H２O犤１０犦。我们用水热法以三乙胺做模板剂获得了一种全新的二帽pse…     

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…     

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…     

Synthesis,Structure and Biological Activities of a Novel Anionic Organotin(Ⅳ) Complex {[(pClC_6H_4CH_2)Sn(H_2O)(Cl)_2OCOCH(O)CH(O)CO_2Sn(H_2O)(Cl)_2(p-ClC_6H_4CH_2)]·2(HNEt_3)}

A novel anionic organotin(Ⅳ) complex {[(pClC_6H_4CH_2)Sn(H_2O)(Cl)_2OCOCH(O)CH(O)CO_2Sn(H_2O)(Cl)_2(p-ClC_6H_4CH_2)]·2(HNEt_3)}(1) was synthesized by the reaction of di(p-chlorobenzy)tin dichloride with the D-tartaric acid in 2:1 molar in the presence of an organic base triethylamine. The structure was characterized by elemental analysis, IR, TG, XRD and single-crystal X-ray diffraction. It crystallizes in triclinic, P1 space group, with a = 0.7067(1), b = 1.9762(3), c = 2.2383(3) nm, α = 91.544(2)°, β = 90.075(2)°, γ = 90.110(2)°, V = 3.1247(7) nm~3, Z = 3, Dc = 1.621 g/cm~3, m(Mo Kα) = 16.29 cm–1, F(000) = 1530, R = 0.0394, wR = 0.1092,(Δρ)max = 1224 and(Δρ)min = –840 e/nm~3. The stabilities, orbital energies and composition characteristics of some frontier molecular orbitals of 1 have been carefully investigated with quantum chemistry calculation. In addition, the in vitro antitumor activity suggested that 1 had stronger inhibitory activity on H460, MCF7 than on A549.     

Hydrothermal Synthesis and Crystal Structure of a New Polyoxovanadate:[Mn(en)_3]_2en_(0.5)[HV_8~ⅤV_8~ⅣO_(38)(Cl)]·4.5H_2O(en=Ethylenediamine)

A new compound has been synthesized under hydrothermal conditions and characterized by IR,elemental analysis,XPS and single-crystal X-ray diffraction analysis. The title compound [Mn(en)3]2en0.5[HV16O38(Cl)]·4.5H2O crystallizes in monoclinic,space group C2/c,with a=17.016(4),b=18.858(4),c=18.872(4),β=93.667(4)o,V=6043(2)3,Z=4,Dc=2.242 g/cm3,Mr=2040.12,F(000)=4020,μ=2.895 mm-1,Rint=0.0921,R=0.0649 and wR=0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38(Cl)]4-cage,two [Mn(en)3]22+ cations,four and a half lattice waters and a half ethylenediamine. In addition,intermolecular O-H···N,O-H···O,N-H···O and C-H···O hydrogen bonds link the molecules together to form a three-dimensional structure.     

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。     

Hydrothermal Synthesis and Crystal Structure of a Highly Reduced Mixed Molybdenum-vanadium Polyoxometalate with Phosphorus-centered [Ni(phen)_3]_2H_2· [PMo_4~ⅤMo_4~ⅥV_6~ⅣM_2M_(44)]~(5-)·4H_2O(M=0.78Mo~Ⅴ+0.22V~Ⅳ)

Introduction Polyoxometalates(POMs)containingKeggin moietiesexhibitawidevarietyofcompositionsand haveconsiderablestructuralversatilityaswellas importantmagnetic,optical,andcatalyticproper- ties[1_6].Itisthereforevitaltodesignandsynthe- sizenovelPOMswithdifferentstructuralcharac- teristicsinordertoexploretheirproperties.Inthe lastfewyears,oneoftheimportantadvancesin transitionmetalchemistryhasbeenthestudyof cappingstructuralpolyoxoanionsandclosinghost cagestructuralmetal-oxygenclustercompoun…     

Synthesis and Crystallographic Characterization of Complex [(CH_3)_3NCH_2CH_2N(CH_3)_3][HgI_4]·H_2O Containing Novel Cation

1 INTRODUCTION The crystal structures of several tetrahalogeno-mercurates (II) have been reported with a wide va-riety of stereochemical arrangements[1, . These stu- 2]dies have shown that the Hg atom…     

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 Characterization of the Chiral Skeleton Cluster [η~5-C_5H_4C(O)CH_2CH_2C(O)OCH_3]RuCoW(μ_3-Se)(CO)_8

1　ＩＮＴＲＯＤＵＣＴＩＯＮＴｒａｎｓｉｔｉｏｎｍｅｔａｌｃｌｕｓｔｅｒｃｏｍｐｌｅｘｅｓｈａｖｅｂｅｅｎｒｅｃｅｉｖｉｎｇｃｏｎｓｉｄｅｒａｂｌｅａｔｔｅｎｔｉｏｎｉｎｒｅｃｅｎｔ ｙｅａｒｓｌａｒｇｅｌｙｂｅｃａｕｓｅｏｆｔｈｅｉｒ ｐｏｔｅｎｔｉａｌａｐｐｌｉｃａｔｉｏｎｓｉｎｃａｔａｌｙｓｉｓａｓｗｅｌｌａｓｔｈｅｎｏｖｅｌｔｙａｎｄｖｅｒｓａｔｉｌｉｔｙｏｆｔｈｅｉｒｒｅａｃｔｉｏｎｓａｎｄｓｔｒｕｃｔｕｒｅｓ.[1～ 4] Ｏｕｒｉｎｔｅｒｅｓｔｉｎｍｅｔａｌｃｌｕｓｔｅｒｃａｔａｌｙｓｉｓｐ…     

Crystal Structure of [CH_3CH(OH)COO]_2Fe(H_2O)_2·H_2O

<正> The title compound C6H16O9Fe, Mr = 288. 13, was synthesized and crystallized in monoclinic space group P21/c, a = 9. 409(4), b = 5. 812(4), c= 22. 122(7)(?) , β=90. 80(3)°. V = 1209. 6(?)3, Z = 4, Dc=1. 572g/cm3, F(000) = 592, μ = 12. 73cm-1, R = 0. 063, Rw= 0. 068 for 1191 observed reflections. The iron atom is surrounded by O(1 - 6) in a distorted octahedron.     

[H_2N(C_2H_4)_2NH_2]_4(H_3O)[PMo_2~VMo_6~(VI)V_4~(IV)O_(40)(V~(IV)O)_2]·H_2O: A New Highly Reduced, Bicapped Pseudo-Keggin Vanadylpolymolybdophosphate

Ｐｏｌｙｏｘｏｍｅｔａｌａｔｅｓ (ＰＯＭｓ)ｃｏｎｔａｉｎｉｎｇＫｅｇｇｉｎｍｏｉ ｅｔｉｅｓｈａｖｅｂｅｅｎｒｅｃｅｉｖｉｎｇｅｘｔｅｎｓｉｖｅａｔｔｅｎｔｉｏｎｉｎｒｅｃｅｎｔｙｅａｒｓｏｗｉｎｇｔｏｔｈｅｉｒｇｒｅａｔｆｕｎｄａｍｅｎｔａｌａｎｄｐｒａｃｔｉｃａｌｉｎｔｅｒ ｅｓｔ .1Ｅｓｐｅｃｉａｌｌｙｔｈｅｕｎｕｓｕａｌｅｌｅｃｔｒｏｎｉｃｐｒｏｐｅｒｔｙ (ｈｉｇｈｎｅｇａｔｉｖｅｃｈａｒｇｅｓ) ,ｏｎｅｏｆｔｈｅｍｏｓｔｉｍｐｏｒｔａｎｔｐｒｏｐｅｒｔｉｅｓｏｆＰＯＭｓ ,ｈａｓｐｏｔｅｎ…     

A Novel Pentadecanuclear Neodymium Cluster: Synthesis and Structure of [Nd_(15)(μ_4-tyr)_(10)(μ_3-OH)_(20)(μ_2-OH)_4(OH)_(10)(μ_2-H_2O)-(H_2O)_(10)][Na(ClO_4)_2]·61H_2O

Inthepastfewyears,nearly50kindsofrareearthcomplexeswithaminoacidswerestructurallycharacterizedl.AllofthesecomplexesweresynthesizedunderpHI--4.Astheaminoacidligandsinthesecomplexesareintheirinnersaltformsandtheandnogroupsareprotonned,theycoordinatewithrareearthionsonlybyusingtheircarboxylgroups.Wehavenoticedthatthedeprotonizationoftheprotonnedaminogroupsisnecessarybeforethenitrogenatomsoftheaminogroupscancoordinatewiththemetalions.BycarefullyadjustingthePHvalueofasolutiontoabout5,wecrystalliz…     

Synthesis,Structure and Electrochemistry of Triruthenium Cluster Complex [Ru_3(μ_3- O)(μ-CH_3CO_2)_6(py)_2(PPh_2py)](PF_6)·CH_2Cl_2

1 INTRODUCTION The transition metal cluster complexes exhi- biting multistep redox processes have attracted more and more attention because of their potential applications in the areas of photonic and electronic devices[1～4]. The oxo-centered carboxyla…