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SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF IN-COMPLETE CUBANE CLUSTER C(MoCu_3S_3) (O)(μ-dtp)(PPh_3)_3] 被引量:1
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作者 陈秋华 黄小荥 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1993年第5期391-396,共6页
A new mixed-metal sulfido incomplete cubane cluster [(MoCuS3) (O) (μ-dtp) (PPh3)3] Cdtp = S2P (OC2H5)2] has been prepared by reaction of (NH4)2MoOS3 with Cu(dtp) (PPh3)2 in dimethylformamide solution. It crystallizes... A new mixed-metal sulfido incomplete cubane cluster [(MoCuS3) (O) (μ-dtp) (PPh3)3] Cdtp = S2P (OC2H5)2] has been prepared by reaction of (NH4)2MoOS3 with Cu(dtp) (PPh3)2 in dimethylformamide solution. It crystallizes in the triclinic space group P1, a = 13.810(5), b = 19. 753(5), c=11. 719(4) A. α=99. 42(2), β=107. 24(3),γ=88. 05(3)°, V = 3012(2)A3, Dc = l. 51g/cm3and Z = 2. Final R=0. 046, Rw = 0. 056 for 7700 unique intensity data(I≥3σ(I)). The central unit [MoCu3S3]3+ can be described as a distorted incomplete cube with one missing corner. The Mo atom is tetrahedrally coordinated by three μ3-S atoms and one terminal O atom. Two Cu atoms are tetrahedrally coordinated whereas the third Cu atom has a highly distorted trigonal environment. The mean Mo - Cu bond length is 2. 752A. The Cu...Cu distances are in the range of 3. 200(1) -3. 740(1) A which are too long to form bonds. 展开更多
关键词 Synthesis Crystal Structure Incomplete Cubane Cluster Mo-Cu-S Cluster
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CRYSTAL STRUCTURE AND REACTIVITY OF (Et_4N) [Mo_3(μ_6-O)-(μ-Cl)_3(μ-OAc)_3Cl_3] 被引量:2
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作者 陈秋华 卢绍芳 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1993年第2期117-123,共7页
(Et4N)[Mo3(μ3-O)(μ-Cl)3(μ-OAc)3Cl3], C14H29Cl6Mo3NO7, Mr = 823.92, triclinic, P1, a = 17. 508(4), b = 19. 602(3), c=8. 091(2)A, α=91. 25(2)°, β= 96. 56(2)°,γ= 83. 61(2)°, V = 2741(1)A3, Z = 4, Dc ... (Et4N)[Mo3(μ3-O)(μ-Cl)3(μ-OAc)3Cl3], C14H29Cl6Mo3NO7, Mr = 823.92, triclinic, P1, a = 17. 508(4), b = 19. 602(3), c=8. 091(2)A, α=91. 25(2)°, β= 96. 56(2)°,γ= 83. 61(2)°, V = 2741(1)A3, Z = 4, Dc = 2.00g/cm3, MoKa (λ=0. 71069A), μ= 19. 44cm-1, F(000) = 1616, T = 23℃, final R = 0. 055, Rw = 0. 068 for 5728 unique intensity data (I≥3σ(I)).The molecule consists of cluster aniorn [Mo3(μ3-O) (μ-Cl)3(μ-OAc)3Cl3]- and cation (Et4N) + . There are two independent molecules in an asymmetric unit whose cluster anions A and B have the same configuration except for some bonding parameters. The cluster core may be described as an equilateral {Mo3} triangle with a capping O atom and three bridging Cl atoms below and above it respectively. In addition, each pair of Mo atoms is bridged by an acetate group and each Mo atom is further coordinated to a terminal chlorine atom. The three Mo - Mo bonds are 2. 587 (2), 2.587(2), 2. 582(2) A for cluster anion A and 2. 587(2), 2.595(2), 2.577 (2) A for cluster anion B. Altogether eight, d electrons occupy the {Mo3} cluster bonding orbitals. 展开更多
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Investigation on Magnetic Properties of Exchange Coupled Transition Metal Complexes──I. Application of the Kambe's Theory
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作者 谢秀兰 Augstin,Lo 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1995年第2期145-150,共6页
Magnetic susceptibility of a series of dinuclear Ⅴ(Ⅳ) . Co(Ⅱ) and Mn(Ⅲ) complexes has been measured in the temperature range of 1. 5 ~300K. The isotropic Heisenberg theory has been applied to study the temperatur... Magnetic susceptibility of a series of dinuclear Ⅴ(Ⅳ) . Co(Ⅱ) and Mn(Ⅲ) complexes has been measured in the temperature range of 1. 5 ~300K. The isotropic Heisenberg theory has been applied to study the temperature-dependent behaviour of the magnetic susceptibility of these complexes and a corresponding program for fitting the experimental results has been set up on a VAX 11/785 computer. Conclusions can be drawn that the three complexes studied are all anti-ferromagnetically coupled with coupling constants -4. 4 , -115. 2 , and - 8. 4 cm ̄(-1) for Ⅴ(Ⅳ) . Co(Ⅱ) ,and Mn(Ⅲ) complexes, respectively. 展开更多
关键词 magnetic susceptibility magnetic exchange interaction anti-ferromagnetic coupling isotropic Heisenberg model theoretical fitting
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Synthesis and Crystal Structure of Dinuclear Copper Cluster Compound [Cu(dtp)PPh_3]_2
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作者 陈秋华 黄建全 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1994年第2期102-104,共3页
The title compound [Cu(dtp) PPh3]2 (dtp=S2,P(OEt)2) was prepared by heating the mononuclear compound Cu(dtp)(PPh3)2 in CH3CN solution.It crystallizes in the triclinic space group P1 with parameters a=9.71 6(5),b=11.02... The title compound [Cu(dtp) PPh3]2 (dtp=S2,P(OEt)2) was prepared by heating the mononuclear compound Cu(dtp)(PPh3)2 in CH3CN solution.It crystallizes in the triclinic space group P1 with parameters a=9.71 6(5),b=11.026(5),c=12.475(4) A.α=78.16(3)°,β=102. 64(4), γ=114.34(4)°,V=1178(1)A 3,Z=1,Dc=1.44 g/cm3,MoKα(λ=0.71069 A) μ=12. 48cm-1,F(000)=528.Final R=0.041.Rω= 0. 052 for 3653 unique intensity data(I≥3σ(I)).The molecule of the title compound can be viewed as a centrosymmetric dimer with two[Cu(dtp)(PPh3)] units,which are bridged by two S atoms belonging to the dtp ligands.The exact planar[Cu2S2] core and two[CuS2P] four-membered rings form a chair conformation.The Cu…Cu distance is 2.991(5) A. 展开更多
关键词 SYNTHESIS crystal structure copper cluster dinuclear compound
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Electron-rich Polynuclear Transition Metal Clusters:Ⅱ.Synthetic and Structural Studies of Some Polynuclear Coinage Metal Cluster Compounds
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作者 洪茂椿 刘汉钦 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1994年第4期316-323,共8页
The syntheses and structures of a novel series of polynuclear coinage metal cluster compounds are discussed. The most fascinating structural characteristic of the Au-Ag alloy clusters with Au_18Ag_19 and Au_18Ag_19 co... The syntheses and structures of a novel series of polynuclear coinage metal cluster compounds are discussed. The most fascinating structural characteristic of the Au-Ag alloy clusters with Au_18Ag_19 and Au_18Ag_19 cores and phosphine ligands, which were prepared by the reduction of mononuclear coinage metal complexes R3PAuX and R3PAgX with NaBH4 in organic solution, is their construction from 13-atom gold-centred icosahedral Au_7Ag_6 building blocks. The structures of the polynuclear coinage metal clusters with R2dtc ligands are variable with either unlimited linear chain or triangular M3 units. 展开更多
关键词 polynuclear coinage metal clusters SYNTHESES icosahedral building blocks linear chain
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Synthesis and Crystal Structure ofα-Mo_4 X S_3( μ-dtp)_3(dtp)_3( X= 0 .6S + 0 .4O)
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作者 卢灿忠 庄鸿辉 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1999年第5期368-372,共5页
The title compound (Mo 4XS 15 P 6O 12 C 24 H 30 ), α Mo 4XS 3( μ dtp) 3(dtp) 3 (X=0.6S+0.4O; dtp= -S 2P〔OEt〕 2), isolated as a prismatic black crystal, was prepared from ethanolic solution of Mo(CO) 6, MoCl 5 and ... The title compound (Mo 4XS 15 P 6O 12 C 24 H 30 ), α Mo 4XS 3( μ dtp) 3(dtp) 3 (X=0.6S+0.4O; dtp= -S 2P〔OEt〕 2), isolated as a prismatic black crystal, was prepared from ethanolic solution of Mo(CO) 6, MoCl 5 and P 2S 5. It crystallizes in triclinic system, space group P1 with a=14.031(4), b=13.372(2), c=16.270(8), α=92.15(2), β = 72.91(3), γ = 95.20(2)°, V = 2905.4(2) 3, Z = 2, D c = 1.82 g/cm 3, M r=1598.93, F(000)=1564.8, λ =0.71069 (Mo Kα ), μ =1.584 mm -1 . The final R=0.058, R w =0.057 for 5016 observed reflections with I≥3.0σ(I ). The structure analysis reveals that the title compound has a 〔Mo 4XS 3〕 core, belonging to the cubane type tetranuclear molybdenum clusters family, with one of its four μ 3 caps being statistically occupied by S and O. Three dtp ligands chelated three μ X capped Mo atoms as terminal ligands, while another three dtp bridged these three Mo atoms and the fourth one, forming an α type cluster compound. 展开更多
关键词 SYNTHESIS crystal structure tetranuclear molybdenum cluster
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Crystal Structure of Di-μ-bromo-tris(triphenylphosphine) Di-silver(Ⅰ)
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作者 朱永宝 黄纪青 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1994年第5期325-328,共4页
A binuclear silver complex,Ag2Br2(PPh3)3·CH2Cl2,Mr=1247.4,monoclinic P21/c,a=16.306(3).b=18.444(3),c=18.807(3),β=111.21(2)°,V=5274.1(4).,Z=4,Dc=1.575 g/cm3,λ(MoKα)=0.71073,μ(MoKα)=24.7cm(-1),F(000)=2480... A binuclear silver complex,Ag2Br2(PPh3)3·CH2Cl2,Mr=1247.4,monoclinic P21/c,a=16.306(3).b=18.444(3),c=18.807(3),β=111.21(2)°,V=5274.1(4).,Z=4,Dc=1.575 g/cm3,λ(MoKα)=0.71073,μ(MoKα)=24.7cm(-1),F(000)=2480,final R=0.071,Rw=0.075 for 5007observed reflections.In the complex,Ag(1)and Ag(2)are bridged by two bromineatoms and coordinated in tetrahedral and trigonal geometries,respectively. 展开更多
关键词 silver complex synthesis crystal structure
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Skeleton Vibrations and Force Constants of [Fe_2Cr(μ_3-O)(glycine)_6(H_2O)_3](NO_3)_7.3H_2O
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作者 张琳娜 Straughan, 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1995年第4期286-292,共7页
The iR and Raman spectra were rrieasured for[Fe_2Cr(μ_3-O)-(glycine)_6 (H_2O)_3] (NO_3)_7. 3H2O in the range of 2000~90 cm ̄-1. The assignment of the main skeleton vibrations was made in comparison with related comp... The iR and Raman spectra were rrieasured for[Fe_2Cr(μ_3-O)-(glycine)_6 (H_2O)_3] (NO_3)_7. 3H2O in the range of 2000~90 cm ̄-1. The assignment of the main skeleton vibrations was made in comparison with related compounds. A simplified model as well as a simplified general valence force field was used in the normal coordinate analysis of the skeleton and a set of force constants has been obtained. The calculated frequencies agree well with the observed ones, with a mean deviation of 1.8% which confirms the assignn: ient of their vibrational spectra. On the basis of the data obtained some discussions were made. 展开更多
关键词 trinuclear carboxylato complex vibrational spectrum force constant
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Synthesis and Structural Characterization of the Complex 〔Et_4N〕_2〔Ni_2(C_2S_4)(C_3S_5)_2〕
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作者 盛天录 吴新涛 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1999年第1期22-26,共5页
The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characteriz... The heteroleptic dmit complex Et 4N 2 Ni 2(C 2S 4)(C 3S 5) 2 has been prepared by the reaction of NiCl 2·H 2O with Na 2dmit, NaSC 2H 4OH in the MeOH solution. The compound has been characterized by X ray diffraction study, IR and UV Vis spectroscopy. Crystallographic data : space group: P2 1/n, a=11.843(2), b=11 079(1), c = 15.404(1) , β=110.33(1)°, V = 1895.1 3, Z=2, D c =1.62 g/cm 3 , μ =17.6 cm -1 , F (000)=956, R=0.052, R w =0.061. In the structure of the title complex, the tto (tto=tetrathioxalato) ligand in bridging form is chelated to two nickel atoms and dmit (dmit=1,3 dithiole 2 thione 4,5 dithiolate) ligands coordinated to nickel atoms. 展开更多
关键词 dinuclear nickel dmit complex SYNTHESIS structure
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Research on Reactivities of Mo Cluster. A Selective Substitution Reaction of the Bridging (dtp) Ligand and Structure of Tetranuclear Molybdenum Cluster Compound [Mo_4S_4(μ-O_2CC_6H_5)_2(dtp)_4]
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作者 庄鸿辉 吴鼎铭 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1995年第4期245-249,共5页
The cluster compound [Mo4S4 (μ-O2CC6H5)2(dtp)4] (dtp = S2P (OEt)2)was obtained by the ligand substitution reaction of tetranuclear molybdenum cluster [Mo4S4(μ-dtp)2(dtp)4] in the mixed solvent of acetone, ethanol an... The cluster compound [Mo4S4 (μ-O2CC6H5)2(dtp)4] (dtp = S2P (OEt)2)was obtained by the ligand substitution reaction of tetranuclear molybdenum cluster [Mo4S4(μ-dtp)2(dtp)4] in the mixed solvent of acetone, ethanol and water in the presence of C6H5CO2Na. It is monoclinic and crystallizesin space group C2/c, Mr =1495. 09, a=12. 175 (5) , b=22. 01 (1) , c=20.875(9) ,β=99. 04(4)°; V=5570(5) ; Z=4; Dc= 1. 78g/cm3;μ(MoKα) = 14. 52 cm-1; F(000) =2984. Final R factor is 0. 066. The result reveals that the [Mo4S4] cluster core and t-(dtp)1ligands are retained and onlyμ-bridged (dtp)1- ligands are substituted by (C6H5CO2)1in the substitution reaction, thus producing the title cluster compound,the structure of which contains two species of bidentate ligand. 展开更多
关键词 substitution reaction Mo cluster crystal structure
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SYNTHESIS, STRUCTURE AND PROPERTIES OF Na_3[V_2O_3(nta)_2]·5H_2O
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作者 吴达旭 雷新建 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1993年第2期79-84,共6页
Compound Na3 [V2O3 (nta )2 ]·5H2O (1) (ntaH3 = N (CH2CO2H)3) has been prepared by reduction of a mixture of (NH4)2[VO(O2)2Cl] and H3(nta) in H2O with Na2S2O4. The compound crystallizes in the triclinic system, sp... Compound Na3 [V2O3 (nta )2 ]·5H2O (1) (ntaH3 = N (CH2CO2H)3) has been prepared by reduction of a mixture of (NH4)2[VO(O2)2Cl] and H3(nta) in H2O with Na2S2O4. The compound crystallizes in the triclinic system, space group P1 with Mr = 685. 2, a = 11. 050(6), b=12. 179(4), c=9. 792 (3)A,α=111.71(2),β= 98. 23(3), γ= 89. 36(2)°, Z=2, V = 1210. 5A3,λ(MoKa) = 0. 71069 A, F(000) = 694 and DC = 1. 880g/cm3. The structure was solved by direct methods and refined by full-matrix least squares to final R and Rw values of 0. 055 and 0. 065, respectively.The structure of the anion can be considered as two [VO(nta)] fragments connected by one μ2-O atom. Each vanadium atom in the fragment is coordinated by one vanadyl oxygen atom, one bridging-oxygen atom, three oxygen atoms and one nitrogen atom from (nta) ligand in a distorted octahedral geometry. In this paper, we have studied the conversion of compound 1 to mononuclear compound Na2[VO(O2) (nta)]·5H2O (2) by oxidation with hydrogen peroxide, as well as their spectro-scopic properties. 展开更多
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Investigation on Magnetic Properties of Exchange Coupled Transition Me
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作者 谢秀兰 徐勇进 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1994年第5期365-370,共6页
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Synthesis and Structural Characterizations of the Heteronuclear Cubane-like Cluster W_2Ag_2S_4(tdt)_2(PPh_3)_2·CH_2Cl_2
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作者 余荣民 卢绍芳 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1996年第5期347-352,共6页
A new heterometallic cluster W2Ag2S4(tdt)2(PPh3)2·CH2Cl2(H2tdt=H2CH3C6H3S2)(Ⅱ) has been prepared from the reaction of a well-defined molecular building block W2S4(tdt)22-(I) with Ag complex. The compound has bee... A new heterometallic cluster W2Ag2S4(tdt)2(PPh3)2·CH2Cl2(H2tdt=H2CH3C6H3S2)(Ⅱ) has been prepared from the reaction of a well-defined molecular building block W2S4(tdt)22-(I) with Ag complex. The compound has been characterized by X-ray diffraction study, IR., UV-Vis Spectroscopy and cyclic voltammetry.Crystallographic data for the compound are: space group P21/n,a=17.234(4), b=17.622(4), c=19. 094(4) A,β= 99. 22(2)°,V=5704(2) A3, Z=4,final R=0. 042 and Rw=0. 049 for 5983 independent reflections with I≥3σ(I) The structure analysis reveals that the cluster contains a cubane-like core [W2Ag2S4]4+ . The coordination geometry of each tungsten atom is a square pyramid just as that in the building block. Two types of metal-metal bonds of W-W bond and W-Ag bond exist in the core. The distance between two Ag atoms is out of the range of bonding. 展开更多
关键词 W-Ag-S cubane-like cluster rational synthesis structure spectrum
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