Crystallographic report: Hydroxytrimethylarsonium iodide, [Me<sub>3</sub>AsOH]I

Patrick, Brian O.; Sun, Hongsui; Fricke, Michael; Cullen, William R.

doi:10.1002/aoc.708

Cited by 2 publications

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References 5 publications

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“…1 H NMR (400 MHz, CD 2 Cl 2 , 293 K): d = 7.2-7.7 (m). 31 In situ NMR experiments. Reactions were conducted in 5 mm OD NMR tubes loaded in a glove box.…”

Section: Methodsmentioning

confidence: 99%

“…The cation has been structurally characterised once before as an iodide salt. 31 The reactions were repeated several times and produced the same products, although the relative amounts of the fluorosilicate anions varied from preparation to preparation. The same products formed when the reaction was conducted in plastic equipment, eliminating the involvement of the glass vessels in the reaction.…”

Section: O-mentioning

confidence: 99%

“…The structure of colourless crystals grown from CH 2 Cl 2 solution showed them to be [Me 3 AsOH] 2 [SiF 6 ] (Fig.6). The cation has been structurally characterised once before as an iodide salt 31. The reactions were repeated several times and produced the same products, although the relative amounts of the fluorosilicate anions varied from preparation to preparation.…”

mentioning

confidence: 99%

“…2 ] identified by in situ31 P{ 1 H} NMR studies, with no resonances attributable to phosphine oxide adducts evident (see experimental section); the systems are also extremely sensitive to moisture. SiHCl 3 and Si 2 Cl 6 are commonly used to convert R 3 PO…”

mentioning

confidence: 99%

“…Found: C, 38.3; H, 8.2%. 1 H NMR (400 MHz, CD 2 Cl 2 , 293 K): d = 1.16 (t, [3H], Me), 1.94 (br, [2H], CH 2 ); no change at 190 K 31.…”

mentioning

confidence: 99%

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Hypervalent neutral O-donor ligand complexes of silicon tetrafluoride, comparisons with other group 14 tetrafluorides and a search for soft donor ligand complexes

et al. 2011

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The hypervalent adducts of SiF(4), trans-[SiF(4)(R(3)PO)(2)] (R = Me, Et or Ph), cis-[SiF(4){R(2)P(O)CH(2)P(O)R(2)}] (R = Me or Ph), cis-[SiF(4)(pyNO)(2)] and trans-[SiF(4)(DMSO)(2)] have been prepared from SiF(4) and the ligands in anhydrous CH(2)Cl(2), and characterised by microanalysis, IR and VT multinuclear ((1)H, (19)F, (31)P) NMR spectroscopy. The NMR studies show extensive dissociation at ambient temperatures in non-coordinating solvents, but mixtures of cis and trans isomers of the monodentate ligand complexes were identified at low temperatures. Crystal structures are reported for trans-[SiF(4)(R(3)PO)(2)] (R = Me or Ph), and cis-[SiF(4)(pyNO)(2)]. The GeF(4) analogues cis-[GeF(4){R(2)P(O)(CH(2))(n)P(O)R(2)}] (R = Me or Ph, n = 1; R = Ph, n = 2) were similarly characterised and the structures of cis-[GeF(4){R(2)P(O)CH(2)P(O)R(2)}] (R = Me or Ph) determined. The reaction of R(3)AsO (R = Me or Ph) with SiF(4) does not give simple adducts, but forms [R(3)AsOH](+) cations as fluorosilicate salts. SiF(4) adducts of some ether ligands (including THF, 12-crown-4) were also characterised by (19)F NMR spectroscopy in solution at low temperatures (∼190 K), but are fully dissociated at room temperature. Attempts to isolate, or even to identify, SiF(4) adducts with phosphine or thioether ligands in solution at 190 K were unsuccessful, contrasting with the recent isolation and detailed characterisation of GeF(4) analogues. The chemistry of SiF(4) with these oxygen donor ligands, and with soft donors (P, As, S or Se), is compared and contrasted with those of GeF(4), SnF(4) and SiCl(4). The key energy factors determining stability of these complexes are discussed.

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“…1 H NMR (400 MHz, CD 2 Cl 2 , 293 K): d = 7.2-7.7 (m). 31 In situ NMR experiments. Reactions were conducted in 5 mm OD NMR tubes loaded in a glove box.…”

Section: Methodsmentioning

confidence: 99%

Section: O-mentioning

confidence: 99%

mentioning

confidence: 99%

mentioning

confidence: 99%

“…Found: C, 38.3; H, 8.2%. 1 H NMR (400 MHz, CD 2 Cl 2 , 293 K): d = 1.16 (t, [3H], Me), 1.94 (br, [2H], CH 2 ); no change at 190 K 31.…”

mentioning

confidence: 99%

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