3878-45-3Relevant articles and documents
Smith, B. C.,Smith, G. H.
, (1965)
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Bartlett,Meguerian
, p. 3710,3714 (1956)
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Smith,Smith
, p. 5514 (1965)
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Chemistry of [CpCr(CO)3]2. Synthesis of Cp2Cr2(CO)4S, Cp2Cr2(CO)4S2, and Cp2Cr2(CO)5S2. Crystal structure and reactivity of Cp2Cr2(CO)4S2 and Cp2Cr2(CO)5S2
Goh, Lai Yoong,Hambley, Trevor W.,Robertson, Glen B.
, p. 1051 - 1057 (1987)
The instantaneous reaction of [CpCr(CO)3]2 (Cp = η5-C5H5) in tetrahydrofuran or toluene with stoichiometric amounts of elemental sulfur produced Cp2Cr2(CO)4S (1) and Cp2Cr2(CO)5S2 (2) in near quantitative yields. A solution of 2 on standing 1 h at ambient temperature gave a mixture of Cp2Cr2(CO)4S2 (3) (76%) and 1. The transformation of the very labile complex 2 to 3 with the cleavage of a CO ligand thence to the linear multiple bonded Cr-S-Cr complex 1 with extrusion of a S atom and finally to Cp4Cr4S4 was demonstrated by a time-dependent NMR study at 30°C. When 2 was treated with CF3SO3CH3, one of the S atoms was immediately methylated, giving [Cp2Cr2(CO)5S2(CH 3)](SO3CF3) (4) as a fine black unstable solid, which decomposed in solution to give 1 and [Cp4Cr4S4(CH3)](SO 3CF3) (5). Complexes 1-3 have been characterized by elemental, spectral, and crystal structure analyses. The structure of 1 has been reported previously. Crystals of 2 are monoclinic, P21/n, with a = 11.638 (4) A?, b = 15.508 (5) A?, c = 9.825 (3) A?, β = 111.56 (2)°, and Z = 4. Crystals of 3 are monoclinic, P21/c, with a = 8.214 (1) A?, b = 11.464 (2) A?, c = 16.182 (3) A?, β = 92.44 (1)°, and Z = 4. The disulfur ligand bridges the two chromium centers asymmetrically μ-η1,η2 in 2 and symmetrically μ-η2 in 3. S-S distances [2.010 (4) A?, 2; 1.990 (1) A?, 3] are similar to those found in other transition-metal μ-S2 complexes. Metal atoms in both complexes exhibit 4:3, 7-coordination.
New Macrocyclic Complexes of Titanum(IV): Synthesis, Reactivity, and X-Ray Crystal Structure of the Trigonal Prismatic Ti(C22H22N4)Cl2, and Synthesis and Reactivity of its Peroxo, Disulphido, and Pyrocatecholato Derivatives
Goedken, Virgil L.,Ladd, Judith A.
, p. 142 - 144 (1982)
The new macrocyclic complex of titanum(IV), Ti(C22H22N4)Cl2 has been shown by X-ray crystallography to have a trigonal prismatic co-ordination geometry; the synthesis and reactivities of the peroxo, disulphido, and pyrocatecholato derivatives are discussed.
Formation of a methine carbon-to-rhenium σ bond in an oxorhenium(V)-benzothiazole complex
Schoultz,Gerber,Hosten
, p. 13 - 16 (2016)
The reaction of trans-[ReOCl3(PPh3)2] with 1-(1,3-benzothiazol-2-yl)-3-benzoylthiourea (Hbbt) in methanol led to the isolation of the complex [ReOCl2(cbt)(PPh3)] (1). It contains the monoanionic bidentate chelate N-((benzothiazol-2-ylamino)methylene)benzamide (cbt). The new ligand cbt is coordinated via a neutral ketonic oxygen and an anionic imino-acyl carbon atom, and was formed by the abstraction of the thionyl sulfur of Hbbt by a triphenylphosphine of the starting complex, with S = PPh3 also been formed as by-product. Compound 1 was characterized by elemental analysis, FTIR, proton NMR and single crystal X-ray diffraction.
Meienberger, Marc D.,Hegetschweiler, Kaspar,Rueegger, Heinz,Gramlich, Volker
, p. 157 - 170 (1993)
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Arbuzov et al.
, (1976)
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Butler,Coville
, p. 59,61 (1977)
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Evidence for the formation of isothiocyanate during sulfurisation of phosphines and phosphites using xanthane hydride
Hanusek, Ji?í,Russell, Mark A.,Laws, Andrew P.,Page, Michael I.
, p. 417 - 419 (2007)
Contrary to a previous report, the sulfurisation of triphenylphosphines and trialkyl phosphites by 3-amino-1,2,4-dithiazole-5-thione (xanthane hydride) does not yield carbon disulfide and cyanamide as the additional reaction products but unstable thiocarbamoyl isothiocyanate which has been trapped with nucleophiles.
Terminal Uranium(V/VI) Nitride Activation of Carbon Dioxide and Carbon Disulfide: Factors Governing Diverse and Well-Defined Cleavage and Redox Reactions
Cleaves, Peter A.,Kefalidis, Christos E.,Gardner, Benedict M.,Tuna, Floriana,McInnes, Eric J. L.,Lewis, William,Maron, Laurent,Liddle, Stephen T.
, p. 2950 - 2959 (2017)
The reactivity of terminal uranium(V/VI) nitrides with CE2(E=O, S) is presented. Well-defined C=E cleavage followed by zero-, one-, and two-electron redox events is observed. The uranium(V) nitride [U(TrenTIPS)(N)][K(B15C5)2] (1, TrenTIPS=N(CH2CH2NSiiPr3)3; B15C5=benzo-15-crown-5) reacts with CO2to give [U(TrenTIPS)(O)(NCO)][K(B15C5)2] (3), whereas the uranium(VI) nitride [U(TrenTIPS)(N)] (2) reacts with CO2to give isolable [U(TrenTIPS)(O)(NCO)] (4); complex 4 rapidly decomposes to known [U(TrenTIPS)(O)] (5) with concomitant formation of N2and CO proposed, with the latter trapped as a vanadocene adduct. In contrast, 1 reacts with CS2to give [U(TrenTIPS)(κ2-CS3)][K(B15C5)2] (6), 2, and [K(B15C5)2][NCS] (7), whereas 2 reacts with CS2to give [U(TrenTIPS)(NCS)] (8) and “S”, with the latter trapped as Ph3PS. Calculated reaction profiles reveal outer-sphere reactivity for uranium(V) but inner-sphere mechanisms for uranium(VI); despite the wide divergence of products the initial activation of CE2follows mechanistically related pathways, providing insight into the factors of uranium oxidation state, chalcogen, and NCE groups that govern the subsequent divergent redox reactions that include common one-electron reactions and a less-common two-electron redox event. Caution, we suggest, is warranted when utilising CS2as a reactivity surrogate for CO2.
Synthesis and stability of sulfur-35 labelled 4-ethylbicyclothiophosphate
Tkachenko,Trofimova,Fedoseev
, p. 973 - 977 (1999)
Different synthetic routes to the preparation of 4-ethyl-2,6,7-trioxa-1-phosphabicyclo[2,2,2]octane-1-thioxide labelled with sulfur-35 have been investigated since it is of considerable interest as radioligand for neurochemistry. The thiophosphate was successfully synthesized by sulfuration of the corresponding bicyclophosphite by elemental sulfur-3 5, however the radiochemical purity of the material obtained in this way proves to be low. Convenient methods for synthesis of the thioxide from [35S] thiourea, based on the results of the autoradiolysis of the starting [35S] thiourea, has been discovered giving rise to thioxide with high radiochemical purity. The autoradiolytic stability of the labelled thiophosphate has been studied. 1999 KluwerAcademic/Plenum Publishers.
Synthesis of Glycosyl Fluorides by Photochemical Fluorination with Sulfur(VI) Hexafluoride
Bannykh, Anton,Khomutnyk, Yaroslav,Kim, Sungjin,Nagorny, Pavel
supporting information, p. 190 - 194 (2021/01/13)
This study describes a new convenient method for the photocatalytic generation of glycosyl fluorides using sulfur(VI) hexafluoride as an inexpensive and safe fluorinating agent and 4,4′-dimethoxybenzophenone as a readily available organic photocatalyst. This mild method was employed to generate 16 different glycosyl fluorides, including the substrates with acid and base labile functionalities, in yields of 43%-97%, and it was applied in continuous flow to accomplish fluorination on an 7.7 g scale and 93% yield.
