Reactions occurring within each one of two mixtures, a mixture of deuterated dimethylsulfoxide, DMSOd 6 , with CH 3 I (system I) and another mixture of DMSO-d 6 with CH 3 I, NaOH and water (system II), were monitored by 1D and 2D nuclear magnetic resonance ( 1 H, 13 C, heteronuclear multiple quantum correlation, heteronuclear multiple bond correlation and diffusion-ordered NMR spectroscopy). The analysis of the spectra as a function of reaction time revealed the formation of methoxybis(trideuteromethyl)sulfonium iodide, 3; the precipitation of hexadeuterated trimethyloxosulfonium, 2a; a methyl exchange between DMSO-d 6 and 2a to produce trideuterated dimethylsulfoxide, DMSO-d 3 , 4, and nona-deuterated trimethyloxosulfonium iodide, 2b; and the production of small quantities of methanol, 5, trideuterated dimethylsulfide, 6, and dimethyl ether, 7, in both systems. Only system II precipitated deuterated [Na 4 (DMSO-d x ) 15 ][(I 3 ) 3 I], 1a, a green solid with metallic shine that corresponds to an isotopomer of 1, which is produced by the self-assembly of DMSO and CH 3 I in the presence of NaOH and water.

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A new complex with the molecular formula [Na(4)(DMSO)(15)][(I(3))(3)(I)] represents the first example of Na(+) coordinated solely by DMSO. The triiodide (I(3)(-)) and iodide (I(-)) anions form an infinite linear chain running throughout the crystal.

The title compound, [Zn{(CH3)2SO}6]I4, is a one-dimensional supra­molecular polymer along a threefold rotation axis of the space group. It is built up from discrete [Zn{(CH3)2SO}6]2+ units connected through non-classical hydrogen bonds to linear I4 2− polyiodide anions (C—H⋯I = 3.168 Å). The ZnII ion in the cation has an octa­hedral coordination geometry, with all six Zn—O bond lengths being equivalent, at 2.111 (4) Å. The linear polyiodide anion contains a neutral I2 mol­ecule weakly coordinated to two iodide ions.