Preparations, structures and reactions of molybdenum complexes of triorgano silylated pyridine-2-thiols

Block, Eric; Gernon, Michael; Kang, Hyunkyu; Ofori-Okai, Gabriel; Zubieta, Jon

doi:10.1021/ic00008a012

Cited by 77 publications

(61 citation statements)

References 2 publications

(3 reference statements)

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“…[69][70][71] The 13 C NMR spectra of the free ligands 4,6-CF 3 MepymSH and 4,6-CF 3 PhpymSH show double the expected number of signals for C(2), C(6), CF 3 and CH 3 , as the free ligands exist in two tautomeric forms. This doubling in the number of signals is not observed in the 13 C NMR spectra of the metal complexes. This situation provides evidence that, in solu-tion, the ligand is coordinated to the metal in the thionate form only.…”

Section: Nmr Spectramentioning

confidence: 76%

“…[1][2][3][4][5][6][7] These latter features are the result of the tendency of thiolate ligands to bridge metal centres to yield oligomeric or polymeric species, a situation that makes it difficult to obtain and isolate crystals suitable for X-ray diffraction studies. It has been shown [8][9][10] that the degree of association depends intimately on both the reaction conditions and the nature of the thiolate ligands. Moreover, these association phenomena may be limited by incorporating steric constraints by appropriate ligand design or introducing coligands to block a number of coordination sites around the metal.…”

Section: Introductionmentioning

confidence: 99%

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Electrochemical Synthesis and Structural Characterisation of Cadmium and Mercury Complexes Containing Pyrimidine‐2‐thionate Ligands

et al. 2005

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The electrochemical oxidation of anodic metal (cadmium or mercury) in a cell containing an acetonitrile solution of the appropriate pyrimidine‐2‐thione (RpymSH) affords complexes [M(RpymS)2] (M = Cd, Hg; R = 4‐CF3, 4,6‐CF3,Me and 4,6‐CF3,Ph). When 2,2'‐bipyridine (bipy) or 1,10‐phenanthroline (phen) was added to the electrolytic cell, adducts of cadmium and compounds with these coligands were obtained. All the compounds have been characterised by microanalysis, IR spectroscopy and, in the case of the compounds that were sufficiently soluble, by 1H, 13C and 199Hg NMR spectroscopy. The compounds [Cd(4‐CF3pymS)2] (1), [Cd(4,6‐CF3MepymS)2(bipy)] (4), [Cd(4,6‐CF3PhpymS)2(phen)] (6) and [Hg(4,6‐CF3MepymS)2] (8) were also characterised by X‐ray diffraction. Compound 1 presents a polymeric structure with the polymer chains interconnected by intermolecular C–H···N interactions. Compounds 4 and 6 adopt mononuclear structures, with weak inter‐ and intramolecular C–H···π interactions, as well as π–π stacking interactions for compound 6. Compound 8 also presents a mononuclear structure with intermolecular π–π interactions between the pyrimidine rings and additional weak Hg···Hg contacts (3.484 Å). (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2005)

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Section: Nmr Spectramentioning

confidence: 76%

Section: Introductionmentioning

confidence: 99%

Electrochemical Synthesis and Structural Characterisation of Cadmium and Mercury Complexes Containing Pyrimidine‐2‐thionate Ligands

et al. 2005

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“…Among the common Cu n clusters (n = 4, [12] 6, [8,9] 7 [13] and 8 [10,11] ) known to be present in Cu-MT, the varied ligation number of the thiolate ion (CysS m , m = 4 to 11) contributes to the diverse stoichiometry that one can anticipate in Cu-MT clusters. Accordingly, many examples of monodentate thiolatocopper(I) clusters have been reported so far by X-ray crystallography [14][15][16] [CuS 2 , [17] CuS 3 , [18,19] Cu 2 S 2 , [20] Cu 3 S 3 , [21] Cu 4 S 4 , [22] Cu 4 S 6 , [18,[23][24][25][26] Cu 5 S 6 , [27,28] Cu 5 S 7 , [29] Cu 6 S 4 (in this work) Cu 7 S 8 , [30] Cu 8 S 8 [31] and Cu 12 S 12 [32] ]. 6 ] (4).…”

Section: Introductionmentioning

confidence: 76%

Flexible Cu^I–Thiolate Clusters with Relevance to Metallothioneins

2007

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“…The Ag 4 (SR) 4 structural unit remains the most common structure observed in Ag-thiolato systems. Depending on R it may exist as a whole or as part of a more complicated structure [51][52][53][54]. Trinuclear complexes are favored over tetranuclear ones when the steric hindrance of the thiol substituent is increased.…”

Section: Resultsmentioning

confidence: 99%

Silver thiolato complexes grafted on silica and dissolved in organic solution

Spennato

Dartiguenave

et al. 2004

Transition Met Chem

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The formation of a covalent, stable, silver-thiolato bond was used to compare the coordination of the silver cation with mercaptopropylsilane molecules grafted on silica and dissolved in organic solvents. The characterization of the homemade BSiLH trap, performed by DRIFT, 29 Si-and 13 C-CP-MAS-n.m.r., showed the presence of a ligand monolayer on the silica surface. This ligand was characterized by its free SAH function. The coordination of Ag + ions was illustrated by the color change of the surface from white to yellow, the disappearance of the SAH vibration and the downfield shift of the carbon atoms located near the S atom. All these changes were also observed for the silver thiolates synthesized in homogeneous medium. Three molecular complexes were isolated as yellow solids and characterized using physicochemical techniques. Monomeric [HNEt 3 ][Ag(NO 3 )L 2 ] (1), tetrameric (AgL 2 ) 4 (2) and trimeric (AgL 3 ) 3 (3) species, each with a linearly coordinated silver cation, were proposed. L 2 H, (MeO) 3 Si(CH 2 ) 3 SH, and L 3 H, N(C 2 H 4 O) 3 Si(CH 2 ) 3 SH, are respectively trimethoxysilyl-and silatranyl-propanethiols. The silver salt and the steric hindrance of the ligand influenced the nuclearity of the molecular silver complexes. Optimization of the BSiLH trapping conditions with pH and time indicated that the best trapping of the Ag + cation was performed for pH values 5-7 and 30 min in batch experiments. Safety discharged waters were obtained after percolation through an BSiLH filled column. The mercaptopropyl-modified silica gel was regenerated with a 1 M thiourea solution at pH 1.

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Preparations, structures and reactions of molybdenum complexes of triorgano silylated pyridine-2-thiols

Cited by 77 publications

References 2 publications

Electrochemical Synthesis and Structural Characterisation of Cadmium and Mercury Complexes Containing Pyrimidine‐2‐thionate Ligands

Electrochemical Synthesis and Structural Characterisation of Cadmium and Mercury Complexes Containing Pyrimidine‐2‐thionate Ligands

Flexible Cu^I–Thiolate Clusters with Relevance to Metallothioneins

Silver thiolato complexes grafted on silica and dissolved in organic solution

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Preparations, structures and reactions of molybdenum complexes of triorgano silylated pyridine-2-thiols

Cited by 77 publications

References 2 publications

Electrochemical Synthesis and Structural Characterisation of Cadmium and Mercury Complexes Containing Pyrimidine‐2‐thionate Ligands

Electrochemical Synthesis and Structural Characterisation of Cadmium and Mercury Complexes Containing Pyrimidine‐2‐thionate Ligands

Flexible CuI–Thiolate Clusters with Relevance to Metallothioneins

Silver thiolato complexes grafted on silica and dissolved in organic solution

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Product

Resources

About

Flexible Cu^I–Thiolate Clusters with Relevance to Metallothioneins