Structure and reactivity of molybdenum clusters with loose coordination site, Mo3[S4P(OEt)2]4L

Huang, J. Q.; Huang, J. L.; Shang, M.; Lu, Shouci; Lin, Xiuping; Lin, Yu-Hua; Huang, M.; Zhuang, Huisheng; Lu, Jun‐Jun

doi:10.1351/pac198860081185

Cited by 67 publications

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“…[2] The mode of coordination of dithiophosphates, (RO) 2 PS 2 -(dtp), is similar to that of diphosphanes, which thus can lead to various complexes of the type [M 3 Q 4 (dtp) 3 L 3 ] + in which L is a neutral donor such as pyridine (py). [7,17] More often the dtp complexes are prepared as carboxylates, [M 3 Q 4 (dtp) 3 (μ-RCOO)L], in which a bridging carboxylate group occupies the sites of two monodentate neutral donors (L), as illustrated in Scheme 1 (the ethoxy groups of dtp are omitted for clarity) for the series of structurally characterized complexes [M 3 Q 4 (dtp) 3 [25,26] of all the transition metals only Cu I has been incorporated. [27,28] A common structural feature of these clusters is a strong preference for the position trans to the capping μ 3 -S atom to be occupied by one sulfur atom from the dtp ligand, whereas the pyridine molecule occupies the position cis to the μ 3 -S atom and trans to the μ 2 -S atom (Scheme 1).…”

Section: Introductionmentioning

confidence: 99%

Cuboidal Mo₃S₄ and Mo₃NiS₄ Complexes Bearing Dithiophosphates and Chiral Carboxylate Ligands: Synthesis, Crystal Structure and Fluxionality

et al. 2011

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New triangular Mo and W cluster complexes incorporating (S)‐lactic acid (HLac), [Mo3S4(μ‐Lac)(dtp)3(py)] (1) and [W3S4(μ‐Lac)(dtp)3(py)] (2), were prepared [dtp = (EtO)2PS2]. Analogous synthetic procedures were adapted for the synthesis of cuboidal Mo3NiS4 to yield [Mo3(Nipy)S4(py)(μ‐OAc)(dtp)3(py)] (3). The crystal structures of 1 and 3 were determined. A detailed variable‐temperature 31P{1H} and 1H NMR study of compounds 1 and 3 indicated fluxional behaviour in non‐coordinating solvents (CDCl3, CD2Cl2 and CDCl2CDCl2). A number of dynamic processes were identified involving the Mo–py site that include configuration inversion [(P) to (M)], hindered Mo–N rotation and pyridine exchange. Experiments with deuterated pyridine revealed a faster substitutional lability of Mo–py compared with Ni–py.

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Section: Introductionmentioning

confidence: 99%

Cuboidal Mo₃S₄ and Mo₃NiS₄ Complexes Bearing Dithiophosphates and Chiral Carboxylate Ligands: Synthesis, Crystal Structure and Fluxionality

et al. 2011

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“…Hence, Ni atoms are only welcome central atoms and Lewis acids for the formation of relatively stable coordination compounds and may not be necessary for the observed organic reactions themselves -at least not in the presence of Pb 2+ ions, and at least not for dimerizations of the nitrile, which have also been observed in the presence of a Mo cluster. [25] To finally elucidate the impact of different chalcogenide anions on the reaction to form 1, we investigated the treatment of NiCl 2 in acetonitrile in the presence of A 2 Ch (A = Li, Na, K; Ch = S, Se, Te) under the same solvothermal reaction conditions. However, no crystalline product could be obtained so far.…”

Section: Resultsmentioning

confidence: 99%

Solvothermal Reactions in and with Nitriles

2015

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“…The concept of quasi-aromaticity of the M03S4 cluster compounds has been developed by the group of Lu (43,44).…”

Section: Electronic Relationship To Fused Ring Hydrocarbonsmentioning

confidence: 99%

Synthesis and Structure of Raft-Type Molybdenum Chalcogenide Clusters

Saito

Imoto

Toko

et al. 1996

ACS Symposium Series

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Tetranuclear molybdenum cluster complexes [Mo4S6X2(PMe3)6] (X = SH, Cl, Br, I, NCS) and [Mo 4 S 6 (dtc)2(PMe3)4] have been synthesized. They have rhombic metal cores of molybdenum atoms in +3.5 oxidation state with 10 cluster valence electrons. Hexanuclear molybdenum cluster complexes [Mo6E8Cl6(PEt3)6] (E = S, Se) with 14 cluster valence electrons form by reduction of the trinuclear cluster complexes with six cluster valence electrons. An intermediate seven-electron cluster complex [Mo3S4Cl3(dppe)2(PEt3)] has been isolated. The X-ray structures of these cluster complexes are described.Chemistry of molybdenum chalcogenide cluster complexes has made a remarkable progress in the last decade with the discoveries of cluster compounds of various types (7-7). A number of compounds with triangular and cuboidal cluster cores are now known but relatively few cluster compounds with raft-type frameworks have been reported. Hie raft structures are built from triangular cores by fusion of the edges. The simplest one is a tetranuclear rhombus and a pentanuclear trapezoid and a hexanuclear parallelogram are also found. Although there have been several examples of such tetranuclear clusters of other metals, there are still a very limited number of molybdenum chalcogenide clusters. The present article is concerned with synthesis and structural characterization of a few tetranuclear and hexanuclear cluster complexes coordinated by trialkylphosphines. Apart of the results have been published previously (28, 29, 35). Tetranuclear Cluster ComplexesSynthesis. The reaction of (NH4)2Mo3Si3 (8) dissolved in butylamine and a THF 0097-6156/96/0653-0240$15. 00/0

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Structure and reactivity of molybdenum clusters with loose coordination site, Mo3[S4P(OEt)2]4L

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Cited by 67 publications

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Cuboidal Mo₃S₄ and Mo₃NiS₄ Complexes Bearing Dithiophosphates and Chiral Carboxylate Ligands: Synthesis, Crystal Structure and Fluxionality

Cuboidal Mo₃S₄ and Mo₃NiS₄ Complexes Bearing Dithiophosphates and Chiral Carboxylate Ligands: Synthesis, Crystal Structure and Fluxionality

Solvothermal Reactions in and with Nitriles

Synthesis and Structure of Raft-Type Molybdenum Chalcogenide Clusters

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Structure and reactivity of molybdenum clusters with loose coordination site, Mo3[S4P(OEt)2]4L

Abstract: Abstract

Cited by 67 publications

References 0 publications

Cuboidal Mo3S4 and Mo3NiS4 Complexes Bearing Dithiophosphates and Chiral Carboxylate Ligands: Synthesis, Crystal Structure and Fluxionality

Cuboidal Mo3S4 and Mo3NiS4 Complexes Bearing Dithiophosphates and Chiral Carboxylate Ligands: Synthesis, Crystal Structure and Fluxionality

Solvothermal Reactions in and with Nitriles

Synthesis and Structure of Raft-Type Molybdenum Chalcogenide Clusters

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Product

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Cuboidal Mo₃S₄ and Mo₃NiS₄ Complexes Bearing Dithiophosphates and Chiral Carboxylate Ligands: Synthesis, Crystal Structure and Fluxionality

Cuboidal Mo₃S₄ and Mo₃NiS₄ Complexes Bearing Dithiophosphates and Chiral Carboxylate Ligands: Synthesis, Crystal Structure and Fluxionality