- Microwave-assisted synthesis of In(SPh)3 and its use as precursor for the self-assembly of two new one-dimensional indium thiolate-dipyridyl compounds
-
Tris(benzenethiolato)indium(III) (In(SPh)3) has been facilely prepared in high yield of 95.0% by a microwave-assisted solvothermal reaction of indium and diphenyl disulphide in methanol in 15 min. The combination of In(SPh)3 as precursor with dipyridyl ligands of bipy (bipy = 4,4′-bipyridine) and dpp (dpp = 1,3-di(4-pyridyl)propane) in methanol at ambient conditions yielded two new compounds, namely In(SPh)3(bipy) (1) and In(SPh)3(dpp) (2), respectively. Single-crystal X-ray crystallographic studies reveal that in both the structures, the five-coordinated In(III) ions in nearly perfect trigonal-bipyramidal geometry are interconnected by the bifunctional dipyridyl ligands to form one-dimensional chains. Their thermal properties have been investigated.
- Li, Jian-Rong,Xie, Zai-Lai,Hu, Bing,Huang, Xiao-Ying
-
p. 265 - 267
(2011/03/20)
-
- On the reactivity of indium(III) benzenechalcogenolates (chalcogen = sulfur and selenium) towards organyl halides for the synthesis of organyl phenyl chalcogenides
-
The reactivity of indium(III) benzenechalcogenolates (chalcogen = sulfur, selenium) towards organyl halides (organyl = alkyl, allyl, benzyl, acyl) was examined. A practical one-pot method to prepare organyl phenyl chalcogenides indium metal and diphenyl dichalcogenide was found. The coupling is fairly broad in scope and generally works better organyl halides capable to produce stable carbocations.
- Peppe, Clovis,Borges De Castro, Lierson
-
p. 678 - 683
(2009/10/30)
-
- Substituent effects on indium-phosphorus bonding in (4-RC6H 4S)3In·PR′3 adducts (R = H, Me, F; R′ = Et, Cy, Ph): A spectroscopic, structural, and thermal decomposition study
-
The tris(arylthiolate)indium(III) complexes (4-RC6H 4S)3In [R = H (5), Me (6), F (7)] were prepared from the 2:3 reaction of elemental indium and the corresponding aryl disulfide in methanol. Reaction of 5-7 with 2 equiv of the appropriate triorganylphosphine in benzene or toluene resulted in isolation of the indium-phosphine adduct series (4-RC6H4S)3In·PR′3 [R = H, R′ = Et (5a), Cy (5b), Ph (5c); R = Me, R′ = Et (6a), Cy (6b), Ph (6c); R = F, R′ = Et (7a), Cy (7b), Ph (7c)]. These compounds were characterized via elemental analysis, FT-IR, FT-Raman, solution 1H, 13C{1H}, 31P{1H}, and 19F (7a-c) NMR spectroscopy, and X-ray crystallography (5c, 6a, 6c, and 7a). NMR spectra show retention of the In-P bond in benzene-d6 solution, with phosphine 31P{1H} signals shifted downfield compared to the uncoordinated ligand. The X-ray structures show monomeric 1:1 adduct complexes in all cases. The In-P bond distance [2.5863(5)-2.6493(12) A] is influenced significantly by the phosphine substituents but is unaffected by the substituted phenylthiolate ligand. Relatively low melting points (88-130°C) are observed for all adducts, while high-temperature thermal decomposition is observed for the indium thiolate reactants 5-7. DSC/TGA and EI-MS data show a two-step thermal decomposition process, involving an initial loss of the phosphine moiety followed by loss of thiolate ligand.
- Briand, Glen G.,Davidson, Reagan J.,Decken, Andreas
-
p. 9914 - 9920
(2008/10/09)
-
- Direct electrochemical synthesis of alkane- and arenethiolato derivatives of indium and thallium
-
The electrochemical oxidation of anodic indium in acetonitrile solutions of thiols RSH (R = C2H5, n-C4H9, C(CH3)2C2H5, C6H5, 2-C10H7, C6F5) has been shown to give thiolato derivatives of indium(I), -(II), or -(III), depending on R and on the experimental conditions. With R = C2H5 or n-C4H9, electrolysis in the absence of oxygen gives the hitherto unreported InSR compounds, while, with R = C5H11 or 2-C10H7, the products are In(SR)2, formulated as the In-In-bonded In2(SR)4. Arenethiols yield In(SR)3, and products of this stoichiometry are always obtained in the presence of oxygen. The structures of these compounds are discussed, as are the reactions of the indium(I) and -(II) species with iodine and certain other oxidizing agents. Corresponding reactions with thallium anodes gave T1SR for all R studied (C6H5, C6H4CH3-o, C6H4CH3-m, 2-C10H7).
- Green, James H.,Kumar, Rajesh,Seudeal, Narace,Tuck, Dennis G.
-
p. 123 - 127
(2008/10/08)
-
- Darstellung und Eigenschaften von Alkyl- und Arylthioindanen
-
The reaction of InPh3 with the thiols C2H5SH, n-C3H7SH, t-C4H9SH, PhSH or PhCH2SH or with the α,ω-dithiols HSCH2CH2SH, HSCH2CH2CH2SH, HSCH2CH2CH2CH2SH and HSCH2SCH2SH in different molar ratios and the reactions of InCl3 with the trimethylsilylorganylsulfi
- Hoffmann, Gerhard G.
-
p. 305 - 318
(2007/10/02)
-
- Reactions of Some Main Group Metals with Diphenyl Disulphide and Diphenyl Diselenide
-
Indium reacts with both Ph2S2 and Ph2Se2 in refluxing toluene to give the compounds In(EPh)3 (E = S or Se) in high yield.Under similar conditions tin gives Sn(EPh)4.Thallium reacts with Ph2Se2 to form Tl(SePh), but does not react with Ph2S2.Neither zinc nor gallium reacts with Ph2S2 or Ph2Se2.With mixtures of Ph2E2 and I2, indium yields the previously unreported InI(EPh)2 compounds.The reactions of In(SePh)3 are those of a typical indium(III) Lewis acid.Possible factors affecting the reactions of metals with Ph2S2 or Ph2Se2 are briefly discussed.
- Kumar, Rajesh,Mabrouk, Hassan E.,Tuck, Dennis G.
-
p. 1045 - 1048
(2007/10/02)
-
- COORDINATION COMPOUNDS OF INDIUM. PART 43. INDIUM(III) DERIVATIVES OF BENZENETHIOL, AND THE CRYSTAL STRUCTURE OF TETRAPHENYLPHOSPHONIUM BROMOTRIS(BENZENETHIOLATO)-INDATE(III), Ph4P
-
In(SPh)3 is readily prepared by the reaction of InCl3 and NaSPh in methanol.The compound is a Lewis acid, forming 1:1 adducts with 2,2'-bipyridine, 1,10-phenanthroline.N,N,N',N'-tetramethylethanediamine, bis(diphenylphosphino)ethane, and dimethylsulphoxide, and 1:2 adducts with pyridine, trimethylamine, and triphenylphosphine.Reaction with R4NX (X=Cl, Br, I) or similar salts gives R4N salts, which are 1:1 electrolytes.The structure of Ph4P has been determined by X-ray methods.The crystals are monoclinic, space group P21/c, with cell dimensions a=9.964(3) Angstroem, b=13.477(3) Angstroem, c=30.359(7) Angstroem, α=98.30(2) deg, Z=4, R=0.0622 for 2924 unique observed reflections.The anion has distorted tetrahedral symmetry In the InBrS3 kernel, In-Br=2.527(2) Angstroem, and In-S(av)=2.450 Angstroem.The vibrational spectra of In(SPh)3 and its derivatives in the region 500-200 cm-1 are discussed.
- Chadha, Raj K.,Hayes, Peter C.,Mabrouk, Hassan E.,Tuck, Dennis G.
-
p. 804 - 809
(2007/10/02)
-