Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound 〔Et_4N〕_2〔Mo_2(CO)_8(SC_6H_4-OCH_3-p)_2〕

１　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｏｕｒｅｆｆｏｒｔｓｔｏｄｅｖｅｌｏｐｔｈｅｌｏｗ－ｖａｌｅｎｃｅＭｏ－ＳＲｃｏｍｐｏｕｎｄｓ,ｗｅｈａｖｅｆｏｕｎｄａｎＭｏ（０）－ｃｏｍｐｏｕｎｄ,〔Ｍｏ２（ＳＲ）２（ＣＯ）８〕２－,ｗｈｉｃｈｉｓｏｂｔａｉｎｅｄｆｒｏｍｔｈｅｒｅａｃｔｉｏｎｏｆＭｏ（ＣＯ）６ｗｉｔｈＲＳ－ｉｎｈｉｇｈｙｉｅｌｄ,ｐｏｓｓｅｓｓｅｓａｎｉｎｔｅｒｅｓｔｉｎｇｔｗｏ－ｅｌｅｃｔｒｏｎｔｒａｎｓｆｅｒｐｒｏｐｅｒｔｙ．Ｎｕｍｅｒｏｕｓｋｉｎｄｓｏｆｄｉｎｕｃｌｅａｒｍｏｌｙｂｄｅ…     

Synthesis and Structure of a Dimolybdenum Carbonyl Compound with Thiolato Bridges 〔Et_4N〕_2〔Mo_2(CO)_8(SC_6H_4-Cl-p)_2〕

１　ＩＮＴＲＯＤＵＣＴＩＯＮＳｔｕｄｉｅｓｏｎＭｏ－Ｓ（ＳＲ）ｃｏｍｐｏｕｎｄｓｈａｖｅａｌｗａｙｓｂｅｅｎａｎａｃｔｉｖｅｒｅｓｅａｒｃｈａｒｅａｂｅ－ｃａｕｓｅｏｆｔｈｅｅｘｉｓｔｅｎｃｅａｎｄｉｍｐｏｒｔａｎｃｅｏｆＭｏ－Ｓ（ＳＲ）ｂｏｎｄｉｎｇｉｎｍｏｌｙｂｄｅｎｕｍｅｎ－ｚｙｍｅｓ〔１〕ｉｎｂｉｏｌｏｇｉｃａｌｓｙｓｔｅｍａｎｄｔｈｅｐｏｔｅｎｔｉａｌａｐｐｌｉｃａｔｉｏｎｔｏｍａｔｅｒｉａｌｓａｎｄｃａｔａｌｙｓｔ〔２〕．Ｉｎｒｅｃｅｎｔｙｅａｒｓ,ｗｅａｒｅｉｎｔｅｒｅｓｔｅｄｉｎ…     

Synthesis and Structure of a New Dinuclear Molybdenum(Ⅰ)Compound with Cyclohexanthiolate Ligand,[Mo_2(SC_6H_(11)_2(CO)_8]

<正>Molybdenum( I )-compound [Mo2(SC6H11)2(CO)8] 1, crystallizes in monoclinic, space group P21/c with a = 9.5863(9), b = 9.4469(9), c = 13.869(1) A, β = 99.697(2)°, V= 1238.1(2) A3, Z = 2,DC= 1.734 g/cm3, μ = 12.23 cm-1 and F(000) = 644. The finalR = 0.0455 and wR = 0.1159 for 1590 observed reflections with I> 2σ(I). 1 possesses a rhombic bimetallic core MoS2Mo with the Mo-Mo bond length of 2.975(1) and Mo-S of 2.485(2) A.     

The Molybdenum(0) Complex 〔Et_4N〕_2〔Mo_2(CO)_6(pys)_2〕(pys=Pyridine-2-thiolato)

１ＩＮＴＲＯＤＵＣＴＩＯＮＲｅｃｅｎｔｒｅｓｅａｒｃｈｏｎａｓｅｒｉｅｓｏｆｄｉｎｕｃｌｅａｒｍｏｌｙｂｄｅｎｕｍ（０）ｃａｒｂｏｎｙｌｃｏｍｐｌｅｘｅｓｃｏｎｔａｉｎ ｉｎｇｔｈｉｏｌａｔｏ ｂｒｉｄｇｅｓｈａｓｌｅｄｔｏｔｈｅｃｏｎｃｌｕｓｉｏｎ...     

Synthesis and Structure of a New Dinuclear Molybdenum(I) Compound with Cyclohexanthiolate Ligand, [Mo_2(SC_6H_(11))_2(CO)_6(CH_3CN)_2]

1 INTRODUCTION The chemistry of complexes containing low-valence molybdenum and tungsten metal atoms hasincreasingly attracted the attention from chemistsand bioinorganic chemists due to their significancefor studying metal enzymes[1～5]. Since the s…     

Synthesis,Structure,Characterization and Electrochemistry of a New Dinuclear W(0)-complex 〔Et_4N〕_2〔W_2(CO)_8(SCH_2COOMe)_2〕

１ＩＮＴＲＯＤＵＣＴＩＯＮＲｅｃｅｎｔｌｙ,ｔｈｅｃｈｅｍｉｓｔｒｙｏｆｃｏｍｐｌｅｘｅｓｃｏｎｔａｉｎｉｎｇｌｏｗ ｖａｌｅｎｃｅｍｅｔａｌａｔｏｍｓｈａｓｉｎｃｒｅａｓ ｉｎｇｌｙａｔｒａｃｔｅｄｔｈｅａｔｅｎｔｉｏｎｆｒｏｍｃｈｅｍｉｓｔｓａｎ...     

Synthesis and Structure of Tungsten Carbonyl Compound with 2-Mercapto Pyrimidine [Et_4N] [W (CO)_4(SC_4H_3,N_2) ]

1INTR0DUCTI0NLowva1encemolybdenum/tungstencomp1exeswiththiolatoligandsareusefulforthestudiesonsyntheticandstructuralchemistry.Inrecentyearswehavesynthe-sizedandcharacterizedaseriesofdinuclearMo-SRc0mpoundscontainingaplanarMoSzMocorewithamon0dentatethiolatoligand"-"anda"butterfly"M0S2Mocorewithabidentatethi0latoligand"=."H0wdoesmultidentateliganddo"hasnaturallyattracted0urinterest-2-mercaptoPyrimidine(PymS)wasusedasamultidentateligandtocarry0utsynthesisexperiment.unexpectedly,whichgavea…     

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

１　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｒｅｃｅｎｔｙｅａｒｓ,ｔｈｅｚｉｎｉｃｃｏｍｐｏｕｎｄｓｃｏｎｔａｉｎｉｎｇｓｕｌｆｕｒａｎｄｎｉｔｒｏｇｅｎａｔｔｒａｃｔｍｏｒｅａｎｄｍｏｒｅａｔｔｅｎｔｉｏｎｂｅｃａｕｓｅｏｆｔｈｅｉｒｄｅｅｐｒｅｌａｔｉｏｎｓｈｉｐｗｉｔｈｂｉｏ－ｉｎｏｒｇａｎｉｃｃｈｅｍｉｓｔｒｙ〔１〕．Ｚｉｎｉｃｓｕｌｆｉｄｅｐｌａｙｓａｎｉｍｐｏｒｔａｎｔｒｏｌｅｄｕｅｔｏｉｔｓｓｉｇｎｉｆｉｃａｎｔｉｎｖｏｌｖｅｍｅｎｔｉｎｔｈｅｓｔｕｄｙｏｆｔｈｅｐｈｏｓｐｈｏｒｓ,ｓｅｍｉ…     

Synthesis and Structure of 〔Cu(μ-C_6H_5COO)_2(C_4H_8O)〕_2

1mTRODUCT1ONBinuclearcoppercomplexesareimportantnotonlyincoordinationchemistryandmagnetostructuralstudiesbutalsoinpracticalapplication.tliInanattempttoseekthedisPersionandemulationreagentsofCWM(themixtureofcoalandwater),thetitlecomP0undwassynthesizedbyanoxidativepreparationmethodt2i,whosesynthesisandstructurearedifferentfromthosedescribedbyWangetoft3i.Here,0nlythesynthesisandstructureofthetitlecomP0undarereportedandthestudiesofitsappli-cationareinprogress.2EXPERIMENTAL2.1Preparati0n…     

Crystal Structure of 〔PdCl_4〕·〔C_4H_(10)NO〕_2 Compound

INTRODUCTIONPalladiumcomplexesplayanimportantroleinmanycatalyticreactions,especial-lyincarbonylationofolefins.InordertostudytherelationshipbetweenthestructureandproPertyofpalladiumcomplexcatalyst,thetitlecomplexwassynthesizedanditsstructurewascharacterizedbyX-raydiffractionmethod.2EXPERmENT2.1SynthesisAmixtureofmorpholine(o-lmol)andCuCl(O.2mol)inmethanol(8OmL)wasrefluxedfor6h.AftercoolingthesolutionwasfilteredrePeat-edlyunti1theclearfiltratewasobtained.BrownCuCl.C'H,NOcrystalswer…     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound[Et4N]2[Mo2(CO)8(SC6H4-CH3-p)2]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｉｎｃｅｔｈｉｏｌａｔｅｌｉｇａｎｄｗａｓｉｎｔｒｏｄｕｃｅｄｉｎｔｏｍｏｌｙｂｄｅｎｕｍｃａｒｂｏｎｙｌｃｏｍｐｏｕｎｄｉｎ1 984 [1],ｔｈｅｉｎｖｅｓｔｉｇａｔｉｏｎｏｎｌｏｗ ｖａｌｅｎｃｅＭｏ -ＳＲｃｏｍｐｏｕｎｄｓｈａｓｒｅｃｅｉｖｅｄａｔｔｅｎｔｉｏｎｆｏｒｔｈｉｓｋｉｎｄｏｆｌｏｗ ｖａｌｅｎｃｅｃｏｍｐｏｕｎｄｓｐｏｓｓｅｓｓｃｅｒｔａｉｎａｄｖａｎｔａｇｅｏｎｃｏｍｐｏｕｎｄｓｙｎ ｔｈｅｓｉｓ,ｍｏｌｅｃｕｌｅｓｔｒｕｃｔｕｒｅａｎｄｐｈｙｓｉｃａｌａ…     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound [Et4N ] 2 [Mo2 (CO) 8 (SC6H4-OCH3-p) 2]

Reaction of Mo(CO)6 with p-H3CO-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2 (CO)8 (SC6H4-OCH3-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C38H54Mo2N2O10S2, Mr = 954.87, triclinic, P-1, a = 11.348 (7), b =11.616(5), c=10.065(7) A, a=113.86(4), β=111.39(5), γ=91.92(5)°, V=1104.0(1) A3, Z=1, Dc=1.44 g/cm3, F(000)=492, μ=7.0cm-1, Final R=0. 046 and Rw=0. 049 for 2657 reflections with I＞3. Oσ(I). The X-ray structure analysis revealed that the Mo2S2 core of 1 is planar. The geometry around each Mo atom is a distorted octahedron, the two octahedrons form an edge-sharing bioctahedron. The bond. In addition, the 95Mo NMR chemical shift of 1 is discussed.     

Synthesis and Structure of a Dimolybdenum Carbonyl Compound with Thiolato-Bridges [Et4N] 2 [Mo2 (CO) 8 (SC6H4-Cl -p) 2]

Reaction of Mo (CO)6 with p-Cl-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum (0) compound [Et4N]2 [Mo2 (CO)8 (SC6H4-Cl-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C36H48Cl2Mo2N2O8S2, Mr= 963.71, monoclinie, P21/c, a=9. 269(4),b=13.750(3), c=17.466(6) A ;β=104.84(3)°; V=2151.8(3) A3; Z=2; Dc=1.49 g/cm3; F(000)=984; μ=8.3 cm-1; MoKα radiation (λ=0. 71073A ); Final R = 0. 055 and Rw=0. 065 for 3287 reflections with I＞3. 0σ(I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distance is 4. 014(2) A , and this obviously indicates the absence of Mo-Mo bond.     

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…     

簇合物[Et4N]2[Mo2S4(SCH2CH2S)2]的合成及晶体结构

以(NH4)2MoS4,Et4NBr,HSCH2CH2SH为原料合成了新的簇合物——[Et4N]2[Mo2S4(SCH2CH2S)2],其结构经X射线四圆衍射仪,IR。UV及元素分析确证。其晶体属单斜晶系。晶胞参数为：a=1．0304(8)nm,b=1．4158(8)sin。c=1．1417(1)nm,V=1．63801nm^3,z=4。晶体结构经块状矩阵最小二乘法修正后,最终偏离因子R=0．084。     

The Molybdenum(0) Complex [Et4N]2[Mo2(CO)6(pys)2](pys=Pyridine-2-thiolato)

The title compound tetraethylammonium hexacarbonylbis(μ-pyridine-2-thiolato-S∶S) dimolybdenum [Et4N]2[Mo2(CO)6(pys)2] crystallizes in the monoclinic, space group, P21/c with a=13.217(2), b=21.648(2), c=27.193(6)(), β=82.52(2)°, V=7714.6()3, Z=8, Mr=840.77, Dc=1.45 g/cm3, μ=7.8 cm-1, R=0.038 and Rw=0.040 for 6082 reflections with I≥3σ(I). X-ray crystal structure study reveals that the asymmetric unit of the title compound is comprised of two independent formulations of the molecular formula. Each dianion has approximate C2 symmetry and the dimetallic Mo2S2 core adopts a "butterfly" conformation with a dihedral angle between the halves of 139.3(1)° for the first independent anion and 142.8(1)° for the second one. The two pyridine rings lie on the same side of the molecule in a cis arrangement and the Mo...Mo separations are 3.76(1) and 3.838(1)().     

簇合物[Et4N]2[Mo2S4(SCH2CH2S)2]的合成及其结构研究

以(NH4)2MoS4,Et4NBr,HSCH2CH2SH为原料,合成出[Et4N]2[Mo2S4(SCH23CH2S)2]簇合物,用X射线衍射法测定了晶胞结构.其晶胞参数为a=1.0304(8)nm,b=1.4158(8)nm,c=1.1417(1)nm,V=1.63801nm3,Z=4,晶体属单斜晶系,晶体结构经块状矩阵最小二乘法修正后,最终偏离因子R=0.089.此外还进行了红外光谱,紫外可见光谱的测定.     

Synthesis and Crystal Structure of Compound [ZnS6 (C12H8N2)]

The title compound ZnS6(C12H8N2) was obtained by reaction of zinic powder with sulfur and 1,10-phenathtroline in DMF solvent, and its structure has been determined by single crystal X-ray diffraction analysis. The crystal data for the compound: triclinic, P-1, Z = 2, a = 8. 159(2), b = 9. 485(2), c = 11. 997(2)A , α =110. 00(3)°,β = 99.22(3)°, γ = 100.57(3)°, V = 832A3, Dc =1. 748g/cm3, μ(MoKa)=0. 2219 cm-1, F(000)=440. The structure was refined to R = 0. 0723 and Rw = 0. 0865 for 1427 independent observed reflections. The tilte crystal consists of a discrete molecules, in which the core of ZnS2N2 shows a distorted tetrahedral geometry.