Synthesis and structure of {Mo_3S_7[S_2P(OC_2H_5)_2]_3}{Mo_3S_4[S_2P(OC_2H_5)_2]_4(SCN)} and interaction between their cluster units

Ｔｈｅｔｒｉｍｏｌｙｂｄｅｎｕｍｃｌｕｓｔｅｒｓｗｉｔｈｇｅｎｅｒａｌｆｏｒｍｕｌａ[Ｍｏ3(μ3Ｓ)(μＳ)3(μｄｔｐ)(ｄｔｐ)3Ｌ](ｄｔｐ=(Ｓ2Ｐ(ＯＣ2Ｈ5)2)-,Ｌ=Ｈ2Ｏ,ｐｙ,ＳＣ(ＮＨ2)2ｅｔｃ.)[1](ｒｅｆｅｒｒｅｄｔｏａｓＭ1ｔｙｐｅ[2]),ａｎｄ[Ｍｏ3(μ3Ｓ)(μＳ2)3(ｄｔｐ)3]Ｘ(Ｘ=Ｃｌ,Ｉ)[3](ｒｅｆｅｒｒｅｄｔｏａｓＭ2ｔｙｐｅ),ａｒｅｔｗｏｍａｉｎｔｙｐｅｓｏｆｔｒｉｍｏｌｙｂｄｅｎｕｍｃｌｕｓｔｅｒｓｅｖｅｒｉｎｖｅｓｔｉｇａｔｅｄｂｙｏｕｒｒｅｓｅａｒｃｈｇｒｏｕｐ.Ａｓｗｅｈａｖｅａｌｒｅａｄｙ…     

Synthesis and structure of a novel MoFe_4S_4 cubane-like cluster (Me_3PhCH_2N)_2[MoFe_4S_4(SC_6H_(11))_7]

Ｉｔｉｓｗｅｌｌｋｎｏｗｎｔｈａｔｉｎｎａｔｕｒｅｔｈｅａｃｔｉｖａｔｉｏｎａｎｄｒｅｄｕｃｔｉｏｎｏｆｄｉｎｉｔｒｏｇｅｎｉｎａｉｒｔｏａｍｍｏｎｉａａｒｅｃａｔａｌｙｚｅｄｂｙｎｉｔｒｏｇｅｎａｓｅａｔａｍｂｉｅｎｔｔｅｍｐｅｒａｔｕｒｅａｎｄｐｒｅｓｓｕｒｅ.ＴｈｅｍａｉｎｃｏｍｐｏｎｅｎｔｓｏｆｔｈｅａｃｔｉｖｅｃｌｕｓｔｅｒｏｆＭｏＦｅｐｒｏｔｅｉｎｉｎｎｉｔｒｏｇｅｎａｓｅａｒｅＭｃｌｕｓｔｅｒ(ＭｏＦｅ7Ｓ9ｃｌｕｓｔｅｒ)ａｎｄＰｃｌｕｓｔｅｒ(Ｆｅ8Ｓ8ｃｌｕｓｔｅｒ)[1].Ｉｎｔｈｅｌ…     

Crystal Structure of Complex （Et4N）[VFe3S4Cl3（CH3CN）3]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｉｎｃｅ1980,ｍａｎｙＶ/Ｆｅ/Ｓｈｅｔｅｒｏｍｅｔａｌｌｉｃｓｕｌｆｕｒｃｌｕｓｔｅｒｃｏｍｐｏｕｎｄｓｈａｖｅｂｅｅｎｒｅｐｏｒｔｅｄ.ＲａｕｃｈｆｕｓｓｅｔａｌｏｂｔａｉｎｅｄｔｗｏｋｉｎｄｓｏｆＶ/Ｆｅ/Ｓｃｏｍｐｏｕｎｄｓ[1]ｕｓｉｎｇ(ＣＨ3Ｃ5Ｈ4)2Ｖ2Ｓ4ａｓａｎｏｒｇａｎｏｍｅｔａｌｌｉｃｌｉｇａｎｄ,ｏｎｅｉｓ(ＭｅＣｐ)2Ｖ2Ｆｅ2(ＮＯ)2Ｓ4ｗｉｔｈａｃｕｂａｎｅｌｉｋｅｓｔｒｕｃｔｕｒｅａｎｄａｎｏｔｈｅｒｉｓ(ＭｅＣｐ)2Ｖ2Ｓ4Ｆｅ(ＮＯ)2ａｎｄ(ＭｅＣｐ)2Ｖ2Ｓ4…     

Synthesis and Structure of Dimolybdenum Carbonyl Thiolate Compound [Et4N]2[Mo2（CO）8（SC6H4—CH3—m）2]

1 INTRODUCTION In 1984, thiolate ligand was successfully introduced into molybdenum carbonyl compound by the reaction of Mo(CO)6 with [Et4N]SR( R = C6H5, But) in a moderate condition[1]. From then on, a series of dinuclear molybdenum(0) carbonyl thiolate compounds have been synthesized and characterized by using a variety of thiolate ligands in our research group. It was found that a planar Mo2S2 unit is in the compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-p)2][2] (2) and a "butterfly" t…     

Synthesis and characterization of a new Mo-Fe-S cluster compound containing MoO_3S_3 unit and mixed-valent Mo atoms [Et_4N]_2[Mo_2Fe(CO)_4(S,O-C_6H_4-1,2)_3Cl_2]

Reaction of [Mo3(CO)7(S,O-C6H4-1,2)3]2- with FeCl2 in MeCN at 60℃ affords a new Mo-Fe-S cluster complex containing MoO3S3 unit and mixed-valeut Mo atoms, [Et4N]2[Mo2Fe-(CO)4(O,S-C6H4-1,2)aCl2] (1). 1 is characterized by elemental analysis, IR, Mossbauer spectra, X-ray photoelectron spectra and mass spectra. And the structure of 1 is suggested as the structure which contains a [Mo(S,O-C6H4-1,2)3] unit of which the two of three sulfur atoms link to a Mo(CO)4-moiety and the three oxygen atoms are coordinated to a FeCl2 ligand.     

Synthesis and Crystal Structure of （Et4N）2[Pd2（mp）2（mpH）2]

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ（Ｅｔ_４Ｎ）_２［Ｐｄ_２（ｍｐ）_２（ｍｐＨ）_２］ＳｈｉＪｉ－Ｃｈｅｎｇ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ；ＷｅｎＴｉｎｇ－Ｂｉｎ；ＤｅｎｇＹｕ－Ｈｅｎｇ；ＣｈｅｎｇＣｈａｎｇ－Ｎｅｎｇ；Ｌｉ?..     

Synthesis and Crystal Structure of Mixed Mo－W Cubane－type Cluster Compound ［Mo_2W_2S_4（μ－OAc）_2（dtp）_3（dtpH）］·CH_2Cl_2

Ｓｙｎｔｈｅｓｉｓ　ａｎｄ　Ｃｒｙｓｔａｌ　Ｓｔｒｕｃｔｕｒｅ　ｏｆ　Ｍｉｘｅｄ　Ｍｏ－Ｗ　Ｃｕｂａｎｅ－ｔｙｐｅ　Ｃｌｕｓｔｅｒ　Ｃｏｍｐｏｕｎｄ　［Ｍｏ_２Ｗ_２Ｓ_４（μ－ＯＡｃ）_２（ｄｔｐ）_３（ｄｔｐＨ）］·ＣＨ_２Ｃｌ_２ＣｈｅｎＱｉｕ－Ｈｕ?..     

[Et_4N]_2[Zn_2(OPh)_2Cl_4]的合成和晶体结构

ZnCl2, PhONa和Et4NCl稨2O在乙腈溶剂中反应合成了一种二核锌配合物[Et4N]2[Zn2(OPh)2Cl4]。X射线衍射结果表明,晶体属单斜晶系,C2/m空间群,晶胞参数 a = 14.1366(2), b=13.6985(5), c=9.3308(3)牛?107.851(2)o, V=1719.92(9)?,C28H50O2N2Zn2Cl4,Mr=721.24,Z=2,Dx=1.393g/cm3,μ(MoKα)=1.732mm—1,F(000)=756, R=0.0552, wR=0.1534, S=1.027。 配合物是由2个阳离子Et4N+和1个阴离子[Zn2(OPh)2Cl4]2—组成。阴离子[Zn2(OPh)2Cl4]2—包含着1个中心Zn2O2菱形平面。配合物中的2个锌原子通过2个苯酚中的氧原子桥连,每个锌原子还与2个氯原子配位形成变形四面体结构。     

CRYSTAL STRUCTURE OF [Et_4N]_2[Mo_2O_2(μ-S)_2(S_2)_2]

<正> [(C2H5)4N]2[Mo2o2S2(S2)2], Mr = 676. 74, monoclinic, P21/c, a = 13.510(2), b = 14.373(2), c=14. 777(3)(?), β = 97.53(2)°, V = 2844.7(9) (?)3, Z = 4, Dc= 1. 58g/cm3, μ(MoKα) = 13.0cm-1, F(000) = 1384, R =0. 033 for 1803 observed reflections. The structure contains discrete [Mo2O2S2(S2)2]2- anions and Et4N+ cations. The two oxygen atoms bonded to the Mo atoms are in cis-form with respect to the Mo2S2 bridging unit, with an average Mo- O distance of 1. 678 (?), The Mo…Mo distance is 2. 832(1)(?).     

STRUCTURE STUDIES OF [Et_4N]_4[Cu_8(i-mnt)_6] (i-mnt=S_2C=C(CN)_2) AND [Me_4N]_4[Cu_5Ag_3(i-mnt)_6]·H_2O

<正> [Me4N]6[Ag6(i-mnt)6].H2O(1),[Et4N]4[Cu8(i-mnt)6](2) and [Me4N]4-[Cu5Ag3(i-mnt)6].H2O(3)(i-mnt=S2C=C(CN)2) were synthesized. The crystal and molecular structure of the complex 1 was reported by us.The structure of the complex 2 was determined from single crystal X-ray diffraction data. [Et4N]4[Cu8(i-mnt)s] 2, Mr=1870.46, monoclinic, P21/n, a=14.724(6), b = 17.228(3), c=15.59(1)A,β= 100.75(7)°,V=3886.3A3;Z = 2,Dc= 1.598 g/cm3. Complex 3 has been characterized by ICP elemental analyses and IR spectrum.     

Synthesis and Structureof［（C_2H_5）_4N］［Mo_3（μ_3－O）（μ－Cl）_3（μ－CH_3CH_2COO）_3Cl_3］

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆ［（Ｃ_２Ｈ_５）_４Ｎ］［Ｍｏ_３（μ_３－Ｏ）（μ－Ｃｌ）_３（μ－ＣＨ_３ＣＨ_２ＣＯＯ）_３Ｃｌ_３］ＺｈｕａｎｇＨｏｎｇ－Ｈｕｉ；ＷｕＤｉｎｇ－Ｍｉｎｇ；ＨｕａｎｇＪｉａｎ－Ｑｕａｎ；ＨｕａｎｇＪｉｎ－Ｌ...     

31~P NMR Studies on Quasi-Aromaticity of Mo_3S_3 Core and Structure of {Mo_3(μ_3-S)_3[μ-SOP(OEt)_2][S_2P(OEt)_2]_3(CH3CN)}*CH_3CN

1INTRoDUCTIoNDuringthisdecade,extensivestudieshavebeendoneontheclustercompoundswithMosS`coret1}.Wehavedevelopedanewmethodtosynthesizeaseriesof[Mo,o.S'-.J' ,n=O,l,2,3,inaqueoussolution(2).BythereactionofaqueousclusterionswithHdtp,weobtainedtheircorrespondingcompoundswhichwerefirst-lysynthesizedbythespontaneousself-assemblymethod.Theseaqueousclusterionsandtheirderivativescoordinatedbyorganicligands,bothinaqueousphaseandnon-aqueoussolution,demonstratedreactiveactivitiestowardsmanytransitio…     

A New Ionic Trimolybdenum Cluster Compound:〔Mo_3S_7(S_2P(iprO)_2)_3〕〔S_2P(iprO)_2〕

1INTRODUCTIoNInthepastdecades,thechemistryofMo-Sclusterscontaininga[Mo,(p,-S)(p-S,),j corehasbeenstudiedtextensively,andmanysuchkindofcompoundshavebeensynthesized.(1'2'3'4iHowever,fewcompoundscontainingadiscreteclus-tercationhavebeenreported.[5iInthispaper,wereportthesynthesisandstructureofthetitlecompound.Thisisanewexampleoftrimolybdenumclustercontainingadiscreteclustercation.2EXPERIMENTALAllmanipulationwerecarriedoutinair.2.1Synthesis0f[M0,S,(S,P(iprO),),jtS,P(iprO),jAmixture…     

CRYSTAL STRUCTURE OF (Et_4N)_3[Mo_2Fe_6S_8(SPH)_9]

<正> Introduction. A series Of Mo-Fe-S complexes with doublecubane structure has been synthesized and identified. Because of the similarity of its extended X-ray absorption fine structure (EXAFS) to that of FeMo cofactor and nitrogenase, suggestion has been made that the doublecubane complexes may serve as models for the Mo site of nitrogenase. Therefore, the investigation of this type of complexes has attracted much attention. By using the similar method of spontaeous self-assembly reaction, and starting from certain kinds of Mo-Fe-S compounds, we have been able to obtain several kinds of compounds, one of which     

Synthesis and structure of a novel MoFe4S4 cubane-like cluster (Me3PhCH2N)2 [MoFe4S4 (SC6H11)7]

A novel (Me₃PhCH₂N)₂[MoFe₄S₄(SC₆H₁₁)₇] cubane-like cluster was obtained from a reaction system including (NH₄)₂MoS₄, FeCl₂ and NaSC₆H₁₁ in methanol, and characterized by X-ray crystallography. The title compound crystallizes in triclinic space group witha = 1.523 1(3), b =1.610 5(3),c = 1.838 3(4) nm, α = 77.18 (3)°, β = 75.17(3)°, γ = 64.60(3)°, and Z = 2. Also included in this paper are the discussions on the variation of the reaction products obtained from the participation of cyclohexylthiolate and on the changes of the structural features of the products. Project supported by the National Natural Science Foundation of China and the Climbing Program—State Key Project for Fundamental Research in China, and Hong Kong Research Grants Council (Earmarked Grant No. CUHK. 311/94p).     

The Synthesis and Crystallographic Characterization of Heterotrimetallic Linear Complex of [Et_4N][ (Ph_3P)_2{CuS_2WS_2Fe} Br_2]

1INTRoDUCTIONMolybdenum(Tungsten)-copper-sulfurandmolydenum(tungsten)-iron-sulfurcompoundshavebeenstudiedextensivelybecauseoftheirconnectionwithbiologicalprocesses[l,2j.Someheterotrimetalliccomplexeshavebeensynthesized,suchas[NEt'jtPh,p)sAgSzMoSzCu(CN))and[NEt'jtPh,P),AgS,MooCu(CN)jt3i,[l(CH,CH,)'j(PPh,)2{AgS2WS2Cu}(CN)jt4i,[(CH,CH2)4j(PPh,)2{AgS,WOCu}(CN)j('3,butheterotrimetal1iccomplexescontainingtungsten,copper,andironatomshaveseldombeenreported.Onecomplexofthiskindha…     

Solid－state Synthesis at Low－heating Temperature and Crystal Structure of a Dinuclear Molybdenum Complex with Oxalate Ligand［Bu_4N］_2［Mo_2O_2（OH）_2Cl_4（C_2O_4）］

Ｓｏｌｉｄ－ｓｔａｔｅＳｙｎｔｈｅｓｉｓａｔＬｏｗ－ｈｅａｔｉｎｇＴｅｍｐｅｒａｔｕｒｅａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆａＤｉｎｕｃｌｅａｒＭｏｌｙｂｄｅｎｕｍＣｏｍｐｌｅｘｗｉｔｈＯｘａｌａｔｅＬｉｇａｎｄ［Ｂｕ_４Ｎ］_２［Ｍｏ_２Ｏ_２（...     

Synthesis, Structural Characterization and Reactivity of Two New Triangular Molybdenum Cluster Compounds: Mo_3Te_7-[S_2CN(CH_2CH_2OH)_2]_3I and Mo_3Te_4Y_3[S_2P( ~iPrO)_2]_3I (Y_3=1.43Te+1.57S)

ＩｎｔｒｏｄｕｃｔｉｏｎＩｎｔｈｅｌａｓｔｔｗｏｄｅｃａｄｅｓｉｎｔｅｎｓｉｖｅｓｔｕｄｉｅｓｈａｖｅｂｅｅｎｃａｒｒｉｅｄｏｕｔｏｎｔｈｅｍｏｌｙｂｄｅｎｕｍ (ｔｕｎｇｓｔｅｎ)ｃｈａｌｃｏｇｅｎｉｄｅｃｌｕｓｔｅｒｓ ,ｒｅｓｕｌｔｉｎｇｉｎｔｈｅｄｉｓｃｏｖｅｒｙｏｆｓｅｒｉｅｓｏｆｍｏｎｏｍｅｒ ｉｃ ,ｐｏｌｙｎｕｃｌｅａｒＭｏ(Ｗ ) ａｎｄＭｏ(Ｗ ) ｈｅｔｅｒｏｍｅｔａｌｌｉｃｃｏ ｍｐｌｅｘｅｓ .Ｔｒｉａｎｇｕｌａｒ ,ｃｕｂａｎｅ ,ｏｃｔａｈｅｄｒａｌａｓｗｅｌｌａｓｈｅｘ ｎｕｃｌｅａｒ…     

Synthesis and structure of (Mo3S7[s2p (OC2H5)2]3) MO3S4[S2P(OC2H5)2]4(SCN) and interaction between their cluster units

The synthesis method and crystal structure of a novel Mo₃ cluster wmpound are reported. The results of structural analysis and the quantum calculation for the entire cluster molecule reveal that though two Mo₃ cluster units, which belong to two different kinds of structural type respectively, show an apparent ionic characteristic, the interaction between them via the bridging S atoms is still quite certain. The relationship between cluster electron counting and stability of the Mo₃ clusters are also primarily discussed. Project supported by the National Natural Science Foundation of China (Grant No. 29333031)     

One—dimensional Anion—chain Containing [Mo2O6（pic）2]^2—Unit Connected by Unclassical Hydrogen Bond

ＩｎｔｒｏｄｕｃｔｉｏｎＤｕｒｉｎｇｔｈｅｐａｓｔｄｅｃａｄｅｓ ,ｔｈｅｄｅｖｅｌｏｐｍｅｎｔｏｆｔｈｅｃｏ ｏｒｄｉｎａｔｉｏｎｃｈｅｍｉｓｔｒｙｏｆｍｏｌｙｂｄｅｎｕｍ(ＶＩ)ｆｏｃｕｓｅｄｏｎｍｅｔ ａｌ ｏｘｙｇｅｎｃｌｕｓｔｅｒｓｃｈａｒａｃｔｅｒｉｚｅｄｂｙｆａｓｃｉｎａｔｉｎｇｓｔｒｕｃｔｕｒａｌ,ｅｌｅｃｔｒｏｃｈｅｍｉｃａｌ,ｃａｔａｌｙｔｉｃ ,ｍａｇｎｅｔｉｃ ,ｍｅｄｉｃｉｎａｌ,ａｎｄｐｈｏｔｏｐｈｙｓｉｃａｌｐｒｏｐｅｒｔｉｅｓ ,1ｗｈｉｃｈａｒｅｏｆｆｕｎｄａｍｅｎｔａｌａｎｄ…