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标题两个化合物是在反应体系(NH4)3VS4/CuX/PPh3/NEt4X(X=Br,Ⅰ)中采用低温固相反应方法得到的,单晶X射线结构分析表明:VS4(CuPPh3)5Br2(Ⅰ)和VS4-(CuPPh3)5I2(Ⅱ)是同构的,其中晶体(Ⅰ)属于单斜晶系,空间群P211/c,Mr=19682,a=20.215(7),b=15.691(4),c=27.345(9)A,β=95.29(3)°,V=8637.0A3,Z=4,Dc=1.51g/cm3,F(000)=3968,μ(MoKa)=24.6cm-1,R=0.078。晶体(Ⅱ)亦属于单斜晶系,Mr=2062.2,空间群P21/c,a=20.1613(2),b=15.9718(2),c=27.7427(3)A,β=96.07(1)°,V=8883.4A3,Z=4,Dc=1.54g/cm3,F(000)=4112,μ(MoKa)=22.0cm-1,R=0.068。簇合物(Ⅰ)和(Ⅱ)的簇芯结构可描述为共面的2个开口的扭曲立方烷,在这两个簇合物中,V原子仍保持反应起始物[VS4]3-中的四面体配位,5个CU原子呈近似的四方锥排列,V原子基本上处于Cu5四方锥底面的中心。其中1个Cu原子为平面三角形配位,另外4个Cu原子为严重畸变的四面体配位。 相似文献
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11NTRODUCTIONThetetrathiometalateanions[MS'j"-(M=Mo,W,V,Reetc.)havebeenshowntoactasligandstoawidevarietyofmetalions[li.Thechemistryof[MoS'j'-and[WS'j'-isbyfarthemosthighlydevelopedbecausesomeofthecubane-typeMoFe3S4clustersarerelevanttothenitrogenase"'andMo-Cuantagonismexistsinruminantst3i.However,[VS'j'hasnotbeendeeplyinvestigatedbecauseitissensi-tivetoairandmoisture.Evenso,theextensivevanadiumbiologicalfunctionhasim-pelledmoreandmorescientiststoprobeintothechemistryofthevanadiumco… 相似文献
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11NTRODUCTIONThetetrathiometalateanionsofseveraloftheear1yd-transitionmetalshavebeenshowntoactasligandstoawidevarietyofmetalionst1i.ThechemistryofFMoS'j'-and[WS'j'isbyfarthemosthighlydevelopedbecauseoftheirutilityasprecursorstolinearandcubane-typeMFe3S'clusters,someofwhich(M=Mo)arerelevanttothenativeMo-Fe-Sclusterofthenitrogenase"'.However,thedeepinvestigationonthecharacterizationof[VS'j'hasbeenhamperedfortheonlyknownisolatecompound(NH'),VS'isextremelyhydrolyticallysensitiveinwater… 相似文献
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V-Cu-S异金属簇合物的研究I. [VS4(CuPPh3)4Br]的合成和晶体结构 总被引:3,自引:0,他引:3
以(NH4)3VS4为起始原料, 用低温固相法合成了标题簇合物, 并测定其晶体结构。晶体属空间群P1, 单胞参数a=1.3139(10), b=2.5113(170, c=1.1800(8)nm,α=93.04(6), β=114.86(5), γ=96.71(7)°, Z=2, μ=21.4cm^-^1, R=0.084。在簇合物中, VS4^3^-保持较严格的四面体构型, 并螯合四个Cu(I)离子连同桥Br^-离子形成具有额外面的立方烷簇骼[VS4Cu4Br]。 相似文献
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1 INTRODUCTIONSince1980,manyV/Fe/Sheterometallicsulfurclustercompoundshavebeenreported.RauchfussetalobtainedtwokindsofV/Fe/Scompounds[1]using(CH3C5H4)2V2S4asanorganometallicligand,oneis(MeCp)2V2Fe2(NO)2S4withacubanelikestructureandanotheris(MeCp)2V2S4Fe(NO)2and(MeCp)2V2S4… 相似文献
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1 INTRODUCTION The reactivities of the thiometalates [MOnS4-n]z- (n=0~2) and their applications in synthetic chemistry are very attractive because they have been shown to act as multi-ligands to a wide variety of metal ions[1]. The chemistry of Mo(W)S clusters derived from thiometalates has been most highly developed[2] for some MoS clusters are closely relevant to biological activities[3,4]. As for thiovanadates, only [VS4]3- species has been used as ligands to coordinate metal at… 相似文献
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StructuralStudiesof[V_2S_6O_2(CuPPh_3)_4(CuMeCN)_2]·2CH_2Cl_2·2PrOHZHANGHan-Hui;YUXiu-Fen;YANGRong-Sheng;ZHENGFa-Kun;HUANGLiao-Yu... 相似文献
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在(NH4)3VS4/CuI/Py反应体系中合成了新化合物 [VS4Cu6(Py)8I3]并测定其晶体结构。该化合物(C40H40N8Cu6I3S4V)属正交晶系, 空间群为Fdd2, 晶胞参数为: a = 29.924(6), b = 13.475(3), c = 25.853(5) , V = 10425(4) ?, Dc = 2.006 g/cm3, Mr = 1573.92, Z = 8, (MoK) = 4.546 mm-1, F(000) = 6048。结构由直接法解出, 用全矩阵最小二乘法修正, 最终偏离因子R = 0.023, wR = 0.069。簇合物分子是由6个带端基配体的Cu沿着四面体单元VS4的6条SS边配位而成, 6个Cu排列成了1个八面体, V基本位于八面体的中心, 整个分子具有C2对称性。 相似文献
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ANovelCluster[V_2(AgPPh_3)_6S_6O_2]·2CH_2Cl_2ContainingaCubane-likeArrayofSixSilverandTwoVanadiumAtoms¥ZhengFa-Kun;HuangJin-Shun?.. 相似文献
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The reaction of [(η5-C5Me5)2Mo2(μ3-S)4(CuCl)2] 1 with Na2S in MeCN produced a trinuclear cluster [(η5-C5Me5)2Mo2(μ3-S)(μ-S)3(CuCl)] 2. 2 crystallizes in the monoclinic system, space group P21/c with a = 15.563(3), b = 8.9547(18), c = 17.846(4) , β = 101.29(3)o, V = 2438.9(9) 3, Z = 4, Dc = 1.878 g/cm3, T = 193(2) K, C20H30ClCuMo2S4, Mr = 689.60, F(000) = 1376, μ(MoKα) = 2.335 mm–1, S = 1.050, R = 0.0305 and wR = 0.0688 for 4033 observed reflections with I > 2σ(I). In the structure of 2, one [(η5-C5Me5)2Mo2(μ-S)2S2] moiety and one CuCl unit are assembled into an incomplete cubane-like [Mo2S4Cu] core framework, in which the Cu center adopts a distorted tetrahedral geometry coordinated by one μ3-S atom, two μ-S atoms and one terminal chloride. The two Mo…Cu contacts are 2.7519(7) and 2.7689(8) , respectively. 相似文献
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C6H11Na, Et4NBF4, FeCl2, (NH4)2WS4在20mL CH3OH溶剂的反应中, 标题簇合物(Et4N)3[W2Fe6S8(SC6H11)6(OCH3)3]被分离得到, 对其进行X-ray 单晶衍射和结构解析。 该化合物属正交晶系,空间群 Pmmn, 晶胞参数 a = 17.370(5), b = 15.986(4), c = 17.858(3), V = 4958.6(6)3, Z = 2,C63H135N3O3S14Fe6W2, Mr = 2134.47, Dc = 1.43g/cm3, F(000) = 2172.0, m(MoKa) = 3.49 mm-1, T = 293(2)K。 采用2966个I > 2.0s (I) 的衍射点对所有非氢原子参数进行结构修正。 得到最后的偏离因子为R = 0.072, Rw = 0.091。 这是一个双类立方烷的结构, 2个单类立方烷的端基金属钨原子通过3个甲氧基桥联。 [WFe3S4] 与 [MoFe3S4]簇核结构比较说明, 两者存在一定的相似性。 相似文献
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11NTRoDUCTIONThecomplexchemistryofthetetrathiometallatestMS,j"-(M=Mo,W,n==2lM=V,n=3)hasbeenextensivelyinvestigatedbecauseofitspotentialutilityinimi-tationofbiologicalsystems"'.Especially,vanadium-containingheterometallicsulfurcomplexesareofinterestasmodelsoftheactivesitesinmetalloenzymestobiomimeticchemistst2'33.Studiesonthiometalateandrelatedmultimetalcomplexeshavebeenmain1yaboutsynthesesandcrystalstructures,butNMRinvestigationswereraret43.SinceNMRspectroscopyrespondstothemagneticpro… 相似文献
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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… 相似文献
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Devoy SM Henderson W Nicholson BK Fawcett J Hor TS 《Dalton transactions (Cambridge, England : 2003)》2005,(16):2780-2787
The reactivity of the metalloligand [Pt2(micro-S)2(PPh3)4] towards a variety of copper(II)-ligand systems has been studied. Reaction of [Pt2(mu-S)2(PPh3)4] with copper(II) halide complexes [CuCl2L](L = 2,2'-bipyridine and 1,10-phenanthroline) gave trinuclear dicationic products [Pt2(mu-S)2(PPh3)4CuL]2+, and the 8-hydroxyquinolinate (hq) complex [Cu(hq)2] gave [Pt2(mu-S)2(PPh3)4Cu(hq)]+, isolated as their BPh4- or PF6- salts. Related cationic complexes with other ancillary amine ligands (1,2-diaminoethane, 1,2-diaminopropane, 1,2-diaminocyclohexane) were obtained by reactions of [Pt2(mu-S)2(PPh3)4] with CuCl2 and the amine. In contrast, reaction of [Pt2(mu-S)2(PPh3)4] with CuCl2 and NH3 in methanol gave the intensely blue methoxy-bridged dicopper complex [{Pt(2)(mu-S)2(PPh3)4Cu(OMe)}2]2+, isolated as its hexafluorophosphate salt. Copper beta-diketonate complexes reacted with [Pt2(mu-S)2(PPh3)4] giving [Pt2(mu-S)2(PPh3)4Cu(beta-diketonate)]+PF6- complexes, with the CH3COCHCOCH3(acac) and CF3COCHCO(2-thienyl)(tta) derivatives characterised by X-ray structure determinations. The local Cu(II) environment ranges from distorted square-planar to an intermediate form of square-planar and tetrahedral. The beta-diketonate derivatives show varying stability towards methanolysis, giving [{Pt2(mu-S)2(PPh3)4Cu(OMe)}2]2+. 相似文献
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应用IR、MS和EPR表征CuCl和NH4Y固态离子交换过程以及制备Cu(I)Y的一些特性。固态离子交换程度依赖于反应温度。和还原Cu(II)Y的方法,固态离子交换是更为有效的制备纯Cu(I)Y的方法。 相似文献
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A binuclear vanadium complex NH4[(VⅣO)2(μ2-O)(nta)2][EuⅢ(H2O)9] was synthesized by reaction of NH3VO3, nitrilotriacetic acid and EuCl3 in one aqueous solution. The crystal X-ray analysis shows that the complex contains one binuclear vanadium anion [(VⅣO)2(μ2-O)(nta)2]4- and one [EuⅢ(H2O)9]3+ cation. The molecules are built up to a three-dimensional supramolecular structure through hydrogen bonding. CCDC: 238716. 相似文献
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Tetranuclear [Cu4I4{(S,S)-iPr-pybox}2] (1) and dinuclear [Cu2Cl-{(S,S)-iPr-pybox}2][CuCl2] (2) copper(I) complexes have been synthesized by reaction of iPr-pybox with CuI and CuCl, respectively. Furthermore, dinuclear [Cu2(R-pybox)2][PF6]2 [R-pybox = (R,R)-Ph-pybox (3), (S,S)-iPr-pybox (4)] and mononuclear complexes [Cu(R-pybox)2][PF6] [R-pybox = (R,R)-Ph-pybox (5), (S,S)-iPr-pybox (6)] have been prepared by reaction of [Cu(MeCN)4][PF6] and the corresponding pybox. The structures of complexes 1-3 have been determined by X-ray diffraction analyses. 相似文献
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由[Mo~3(μ~3-O)(μ-S)~3(dtp)~4(H~2O)和PbI~3^-在咪唑存在下反应获得异四核混合簇[Mo~3(PbI~3)S~4(dtp)~3(C~3H~4N~2)~3][(CH~3)~2CO]~2(2)[dtp=S~2P(OC~2H~5)~2^-]。簇合物属斜方晶系,空间群P~b~c~a(No.61),晶胞参数为a=2.3590(3),b=1.9161(5),c=2.6458(9)nm,V=11.959(6)nm^3,Z=8。结构最终偏离因子R=0.067。此四核簇分子具有[Mo~3PbS~4]类立方烷簇芯,簇分子整体对称性接近C~3~v。在同一不对称单元中,簇分子的咪唑环以(NH)和溶剂丙酮分子的氧原子形成O---H---N氢键。 相似文献
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新型六核双网兜状簇合物[MoS4Cu5Br3(Py)7]的合成与晶体结构 总被引:1,自引:0,他引:1
以(NH4)2[Mo2S12]?H2O与过量CuBr在吡啶溶液中反应,得到了一个新型六核Mo/Cu/S簇合物[MoS4Cu5Br3(Py)7]。X-射线单晶结构分析表明它属于三斜晶系,空间群为P?C35H35Br3Cu5MoN7S4,Mr=1335.37,a=11.6274(4),b=12.0127(4),c=18.8872(5),a=82.46(2),b=73.25(2),g=62.800(13),V=2246.8(2)?,Z=2,F(000)=1300.0,Dc=1.974g/cm3,?=5.482mm-1,5718个独立可观察点(I>3(I)),最终偏离因子R和Rw分别为0.042和0.048。标题化合物是由2个相似的网兜状MoS3Cu3簇核通过共用MoSCuS平面形成的双网兜状结构,Mo…Cu距离在2.6830(11)~2.741(2)胖洹? 相似文献