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The triangular six-electron cluster complex [Mo3S4Cl4(PEt3)
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(thf)5] produced by the excision reaction of Mo3S7Cl4 with triethypholsphine is reduced by magnesium at – 20°C. Subsequent addition of dppe (=1,2-his(diphenylphosphino)ethane) to the reduced species affords a seven-electron triangular cluster complex [Mo3S4Cl3(dppe)2(PEt3)]. The complex crystallizes in the space groupCm witha=17.170(6),b-19.878(6),c = 13.289(5) = 121.73(2)°,V = 3858(2) A3, andZ = 2. The structure shows an almost equilateral triangle of three molybdenum atoms capped by a Sulfur atom and bridged by three sulfur atoms. The Mo Mo distances, ranging from 2.804(1) to 2.809(1) A are elongated ca. 0.04 A as compared with lose of a six-electron cluster complex with drape ligands. Two molybdenum atoms have a chlorine and a dppe ligands, and the other molybdenum atom bas a chlorine and a triethylphosphine ligands. The UV-Vis spectrum has a characteristic broad hand centered at 1410 n m, which is not observed for six-electron clusters. The ESR spectrum indicates the presence of an unpaired electron consistent with the formulation of the compound as a seven-electron cluster.Dedicated to Professor fiaxi Lu on the occasion of his 80th birthday. 相似文献
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The metathetical reactions between SnBr4 and Li2[E'C(PPh2E)2] in toluene produce the homoleptic tin(IV) complexes Sn[E′C(PPh2E)2]2 [E = E′ = S ( 1b ); E = S, E′ = Se ( 1c )], which were isolated as red crystals and structurally characterized by X‐ray crystallography. The metrical parameters of these octahedral complexes are compared with those of the all‐selenium analog Sn[E′C(PPh2E)2]2 (E = E′ = Se, 1a ), which was prepared previously by a different route. 相似文献
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Emmanuel Cadot Bernadette Salignac Sabine Halut Francis Scheresse 《Angewandte Chemie (International ed. in English)》1998,37(5):611-613
The pH-dependent self-condensation of the [Mo 2 S 2 O 2 ] 2+ complex fragment gives the wheellike Mo12 cluster depicted on the right (ball-and-stick model; large balls: S, medium balls: O, small balls: Mo). Applying this synthetic strategy to other starting materials could provide access to other polyoxothiometalates with well-defined cavities. 相似文献
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Reaction of [{Cp(CO)3Mo}2SbCl] with S8 or Se8 leads to the formation of cluster compounds [{Cp(CO)2Mo}2ESbCl] (E = S, Se). [{Cp(CO)2Mo}2SSbCl] crystallizes monoclinic, space group P21/n with a = 812.28(3), b = 855.65(4), c = 2441.01(9) pm and β = 90.149(3)°; [{Cp(CO)2Mo}2SeSbCl] · CH2Cl2 crystallizes triclinic, space group P$\bar{1}$ with a = 828.82(9), b = 1002.8(1), c = 1340.0(2) and α = 109.24(1), β = 100.87(1), γ = 96.81(1)°. For both compounds X‐ray crystal structure analysis reveals tetrahedral Mo2SbE cluster cores with Sb–E bond lengths of 256.8(1) pm (E = S) and 265.3(1) (E = Se). According to the 18 electron rule the [{Cp(CO)2Mo}2ESbCl] clusters can be regarded as complexes of the 4 electron donator ESbCl that is coordinated “side‐on” to a {Cp(CO)2Mo}2 fragment. 相似文献
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Lee VY Miyazaki S Yasuda H Sekiguchi A 《Journal of the American Chemical Society》2008,130(9):2758-2759
Group 14 and 16 hybrid heavy bicyclo[1.1.0]butanes (tBu2MeSi)4Si3E (E = S, Se, and Te) 2a-c have been prepared by the [1 + 2] cycloaddition reaction of trisilirene 1 and the corresponding chalcogen. Bicyclo[1.1.0]butanes 2 have exceedingly short bridging Si-Si bonds (2.2616(19) A for 2b and 2.2771(13) A for 2c), a phenomenon explained by the important contribution of the trisilirene-chalcogen pi-complex character to the overall bonding of 2. Photolysis of 2a and 2b produced their valence isomers, the heavy cyclobutenes 3a and 3b, featuring flat four-membered Si3E rings and a planar geometry of the Si=Si double bond. The mechanism of such isomerization was studied using deuterium-labeled 2a-d6 to ascertain the preference of the pathway, involving the direct concerted symmetry-allowed transformation of bicyclo[1.1.0]butane 2 to cyclobutene 3. 相似文献
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Bei-Sheng Kang Ting-Bin Wen Xiang-Yang Yu Hua-Xin Zhang Ye-Xiang Tong Cheng-Yong Su Zhong-Ning Chen Han-Qin Liu 《Journal of Cluster Science》1999,10(3):429-443
Two new members of the hexanuclear series [Co6S8(PR3)6]
n+, complexes [Co6S8(PMe2Ph)6](ClO4) (1) and [Co6S8P(OMe)3
6] (2), have been synthesizes and characterized by X-ray diffraction analyses. Their formation process was postulated to go through trinuclear 3--S bridged moieties. The structural characteristics of the M6E8P6 skeleton of a whole series of [M6E8(PR3)6]
n+ (M=Co, Cr, Fe, Mo; E=S, Se, Te) complexes are presented in terms of atomic distances and core volumes. 相似文献
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Dr. Franziska Gruber 《无机化学与普通化学杂志》2012,638(10):1579-1579
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《Solid State Sciences》1999,1(7-8):497-508
A dodecanuclear cluster complex of chromium [Cr12S16(H)2(PEt3)10] was prepared by the reaction of a hexanuclear cluster complex [Cr6S8(H)(PEt3)6] with elemental sulfur, and characterized by the FAB mass spectroscopy and single-crystal X-ray structure analysis. Crystallographic data: [Cr12S16(H)2(PEt3)10] · 2CH2Cl2 (207 K), triclinic, P1, a = 14.697(6) Å, b = 14.733(5) Å, c = 14.238(5) Å, α= 96.60(3)°, β= 109.77(3)°, γ= 65.69(3)°, Z= 1. This complex contains two octahedral Cr6S8 cluster cores linked by a Cr-Cr and two Cr-S bonds, and each core holds an interstitial hydrogen atom. The intercluster bonding mode is similar to those in the superconducting Chevrel-Sergent phases. The paramagnetic moment of the dodecanuclear cluster decreases remarkably at lower temperatures showing the antiferromagnetic coupling between the paramagnetic cluster centers. 相似文献
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New cadmium chalcogenide cluster molecules [Cd10E4(E'Ph)12(PnPr3)4], E = Te, E' = Te ( 1 ) and [Cd10E4(E'Ph)12 (PnPr2Ph)4] E = Te, E' = Se ( 2 ); E = Te E' = S ( 3 ); E = Se, E' = S ( 4 ) have been synthesized and structurally characterized by single crystal X‐ray structure analysis. The influence of the variation of the chalcogen atom is investigated by structural means and by optical spectroscopy. All cluster‐molecules have a broad emission in the blue‐visible range at low temperature as indicated by photo luminescence (PL) measurements. A clear classification of the emission peak position can be made based on the E' species suggesting that the emission is assigned to transitions associated with the cluster surface ligands. Photoluminescence excitation and absorption measurements display a systematic shift of the band gap to the higher energies with the variation of E and E' from Te to Se to S, as also occurs in the respective series of the bulk semiconductors. 相似文献
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A structural investigation on single crystals of MyMo6Se8 Chevrel phases (M=3d: Ti, Fe, and Co) has been carried out. These latter compounds as well as others with Cr, Mn, and Ni atoms make part of a new original family of Chevrel phases. The M ions occupy new interstices in the tridimensional channels network never observed in the other classical Chevrel phases as Liy, Cuy Mo6X8. They occupy only cavity 2 centered on
and with a progressive delocalization of the M cation versus the nature of the cation from the center of the cavity to the outside . The position in cavity 2 is different from the position of the Cu (2) atoms, the second position of the copper atoms in the channels of the CuyMo6X8 compounds. This new position reinforces the interaction with the Mo6 cluster, and may be able to involve new remarkable physical properties as thermoelectric properties. 相似文献