The preparation of long-chain symmetric di-n-alkyl disulfides based on the reaction of Burns SALTS (RS2O3Na) with iodine is reported.H-1-NMR, FT-IR, and FT-RAMAN spectra of the solid and liquid/molten aliphatic title disulfides were recorded. An assignment of the vibrational frequencies is proposed especially in regard to the S-S and C-S vibrations. Distinct spectral differences are determined between the solid and liquid state, as well as between disulfides with even and those with odd numbered alkyl substituents, respectively. The observed phenomena are ascribed to different species in the solids and liquids/melts and their respective VAN DER WAALS interactions.In addition, mass spectra, GC-MS studies, as well as the thermal behaviour of the disulfides, based on investigations by DSC and TGA, are reported.

The thermal reaction of elemental mercury with diorganvl disulphides (RSSR: R = CH3 and C6H5) has been studied. The corresponding mercury dithiolates (CH3S)2Hg (1) and (C6H5S)2Hg (2) are formed under redox conditions. Heating of 2 in n-octanethiol leads to the formation of the corresponding mercury di-n-octanethiolate (3). Compounds 1, 2, and 3 have been characterized by means of 1H NMR. IR. DSC and DTG methods.

The smallest folding angle yet to be found of a four membered gallium-heteroatom ring system with butterfly geometry is in the title compound [iPr2GaP(iPr2)]2 (II). The synthesis of this compound and of its arsenide homologue (III) via the reaction of iPr3Ga with the H-acidic compounds iPr2EH (E  P, As) is reported. Both compounds react below the decomposition temperature of 400°C, splitting off propene and propane, respectively. They may be suitable organometallic precursors for III/V-layer compounds. On the other hand, the reaction of iPr3Ga with tBu2AsH leads only to the formation of the corresponding Lewis acid-base adduct iPr3Ga·.As(H)tBu2 (IV). Spectra and some physical and chemical properties of the new compounds II–IV are reported.

AbstractWith respect to the reactivity of the Ga‐C, Ga‐Br, and Ga‐E bonds the title reaction is investigated.

The synthesis of tris-i-propylgallan as well as the hitherto unknown bis-i-propylgallium halides and i-propylgallium dihalides are given. The reactions of some of the i-propylgallium derivatives with H-acidic compounds of main-group V and VI of the periodic table are investigated, the reaction products are discussed. Spectra as well as some chemical and physical properties of the new compounds are reported.

ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTReactivity of bromodiisopropylgallium with ethanethiol and ethaneselenol. Synthesis of iso-C3H7(Br)GaEC2H5 (E = S, Se)Gerhard G. Hoffmann and Roland FischerCite this: Inorg. Chem. 1989, 28, 22, 4165–4167Publication Date (Print):November 1, 1989Publication History Published online1 May 2002Published inissue 1 November 1989https://pubs.acs.org/doi/10.1021/ic00321a025https://doi.org/10.1021/ic00321a025research-articleACS PublicationsRequest reuse permissionsArticle Views45Altmetric-Citations8LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InRedditEmail Other access optionsGet e-Alertsclose Get e-Alerts

AbstractThe metal trihalides (I) react with the silyl sulfides (II) to give the thiolates (III).

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 trimethylsilylorganylsulfides (CH3)3SiSC2H5 or (CH3)3SiSPh in different molar ratios, and the reactions of phenylindium diiodide PhInI2 with the thiols CH3SH, C2H5SH, i-C3H7SH or t-C4H9SH have been investigated. The resulting reaction products are described. The results are compared with those of the analogous reactions of the corresponding aluminium and gallium compounds.

The reactions of the aluminium halides AlCl3, AlBr3, and AlI3 (I, II, III) with the trimethylsilylorganylsulfides (CH3)3 SiSCH3, (CH3)3 SiSC2H5, and (CH3)3 SiSPh (IV, V, VI), as well as the lead bis(thiolates) Pb(SCH3)2, Pb(SC2H5)2, Pb(S-i- C3H7)2, and Pb(SPh)2 (XV, XVI, XVII, XVIII) and the redox reactions between III and the organic disulfides CH3SSCH3 and PhSSPh (XXIX, XXX) have been investigated. In benzene solution the reactions of I, II and III with IV, V and VI yield the 1:1 adducts, the aluminium trihalide · trimethylsilylorganylsulfides VII–XIV. By heating under vacuum these adducts form the corresponding organylthioaluminium dihalides. These compounds are obtained as well by the reaction of I, II, and III with XV, XVI, XVII and XVIII. The redox reactions between III and the disulfides XXIX and XXX also lead to the corresponding organylthioaluminium diiodides.

AbstractDie Galliumhalogenide GaBr3 und GaI3 reagieren in benzolischer Lösung mit Bleibis‐(thiolaten) je nach eingesetztem molaren Verhältnis unter Bildung der feuchtigkeitsempfindlichen Produkte (I)‐(III).

Different synthetic routes for the preparation of diiodo(methylthio)gallane are given. Some reactions of this compound with Lewis bases, such as O(CH3)2, S(CH3)2, S2(CH3)2, N(CH3)3, P(CH3)3, and other compounds, such as CH3I, CH3OH, C2H5OH, C2H5SH, i-C3H7SH, and C2H5SeH are investigated. Spectra and some physical and chemical properties of the new compounds are reported. The structure of diiodo(methylthio)gallane is discussed in view of some interesting differences of this molecule in solution and in crystal form.

Abstract′Al‐ und Ga‐trihalogenide (I) reagieren mit den Thiolen (II) in Benzol zu den Komplexen (III).

The reaction between dibromo- or diiodo(methyl)gallane and the trimethylsilyl sulphides (CH3)3SiSR (R = CH3, C2H5, n-C3H7, i-C3H7. Ph, CH2Ph) have been investigated. Halo(methyl)- (organylthio)gallanes are formed. These compounds and their chloro analogues can also be obtained by the reactions between the dihalo(methyl)gallanes and the corresponding leaddi- (thiolates) in the molar ratios 2:1, or from the halo(dimethyl)gallanes and free thiols. Some physical and chemical properties of the new compounds are given, and the tentative mechanisms of these reactions are discussed. Syntheses of methylgalliumdiiodide and dimethylgalliumhalides via trimethylgallane und galliumtrihalides or methylgalliumdihalides are described.

Die Trihalogenide des Aluminiums AlCl3, AlBr3 und AlI3 (1, 2 und 3) sowie des Galliums GaCl3, GaBr3 und GaI3 (4, 5 und 6) reagieren mit einer Reihe von Thiolen RSH (RCH3, C2H5, n-C3H7, i-C3H7, Ph) (7 – 11) in Benzol unter Bildung ihrer Komplexe 12 – 34. Mit den Indiumhalogeniden InCl3 (35) und InI3 (36) konnten dagegen bisher keine analogen Anlagerungsprodukte in Substanz erhalten werden, aber im Falle von 36 1H-NMR-spektroskopisch nachgewiesen werden. Darüber hinaus konnten die bisher unbekannten H2S-Komplexe 40 – 42 von 4 – 6 isoliert werden. 5 und 6 bilden auch mit Selenolen RSeH (RC2H5, i-C3H7, n-C4H9) (43 – 45) eine Reihe stabiler Addukte (46 – 49). Spektroskopische Daten sowie einige chemische und physikalische Eigenschaften der neuen Verbindungen werden mitgeteilt. Complexes from the Trihalides of Aluminium and Gallium with Thiols, Hydrogen Sulfide, and Selenols Trihalides of aluminium (1, 2, and 3) as well as gallium (4, 5, and 6) react with a great variety of thiols RSH (7 – 11) in benzene to form the corresponding complexes 12 – 34. In contrast, analogous addition compounds of the indium trihalides 35 and 36 cannot yet be isolated, but 1H NMR spectra of the reaction mixtures of 36 give evidence for these compounds in solution. Moreover, the hitherto unknown H2S complexes 40 – 42 of 4 – 6 can be isolated. 5 and 6 and the selenols 43 – 45 afford the stable adducts 46 – 49. Spectra as well as some physical and chemical properties of the new compounds are reported.

AbstractPhenylgalliumdiiodid und Methylgalliumdiiodid reagieren mit Alkyl‐ und Arylthiolen unter Bildung der entsprechenden Diiodalkylthio‐ bzw. Diiodarylthiogallane. Bei den Umsetzungen von Methylgalliumdiiodid kann das primär gebildete Addukt sowohl 1H‐NMR‐ als auch IR‐spektroskopisch nachgewiesen werden; es ist sogar möglich, einige dieser Addukte kurzzeitig in Substanz zu fassen. Die 1H‐NMR‐Spektren einiger Thiogallane deuten auf ein interessantes strukturelles Phänomen hin. IR‐Spektren und Molmassen sind angegeben.

Triphenylgallane reacts with alkyl- and aryl-thiols, respectively, with formation of the corresponding diphenylalkyl- and diphenylaryl-thiogallanes. Spectra and some physical and chemical properties of the new compounds are given. The results of the X-ray structure determination of diphenylethylthiogallane are discussed.