N,N,N-Trimethyl-N-(methyl 5-de-oxy-2,3-O-iso-propyl-idene-ß-d-ribo-furan-osid-5-yl)ammonium 4-methyl-benzene-sulfonate sesquihydrate.

The structure of the title compound, [C12H24NO4][C7H7O3S]·1.5H2O, contains alternating layers parallel to (001) of hydro-phobic and polar character, stabilized by C-H⋯O hydrogen bonding. The furan ring adopts an envelope conformation with the C(OMe) atom as the flap, and the dioxolane ring is twisted about one of the O-C(methine) bonds. A comparison to related compounds is presented. The tosyl-ate-O atoms were disordered over two positions with the major component having a site occupancy factor = 0.566 (12). The structure was refined as a rotary twin with regard to rotation about the c axis with the contribution of the second component being 0.0048 (6). Solvate water mol-ecules are highly disordered and were removed using the SQUEEZE procedure; the unit cell characteristics take into account the presence of the disordered solvent. High-resolution (1)H and (13)C NMR spectroscopic data are also presented.

Bis(3,5-dimethyl-pyridine-κN)bis-(tri-tert-butoxy-silanethiol-ato-κS)chromium(II) toluene solvate.

In the title chromium silanethiol-ate, [Cr(C(12)H(27)O(3)SSi)(2)(C(7)H(9)N)(2)]·C(7)H(8), the Cr(II) atom is coordinated by two S and two N atoms in a distorted square-planar geometrical arrangement. The mononuclear mol-ecule lies on a twofold axis that passes through the pyridine N atoms. The toluene solvent mol-ecule is equally disordered about a twofold axis.

A study of chirality in bis(1,2-dimethoxyethane-kappa2O,O')sodium bis(tri-tert-butoxysilanethiolato-kappa2O,S)sodate.

This work presents an analysis of self-assembly of a complex molecule from simpler ions, some of which are asymmetric, and is an example of a sodium silanethiolate. The tri-tert-butoxysilanethiolate anion has two helical conformers (P and M), so aggregation of silanethiolates can proceed with recognition of chirality. Alkali metal silanethiolates can form cyclic solvated oligomers (e.g. dimers) or complexes such as sodates with anions of general formula R2Na(-). We note that all known sodates (and lithiates) contain both ligands of the same helicity in the anion, whereas in the dimers the metal atoms are coordinated by silanethiolate ligands of different helicity. The title compound, a new example of a sodate, [Na(C4H10O2)2][Na(C12H27O3SSi)2] or [Na{((t)BuO)3SiS}2][Na(DME)2] (DME is 1,2-dimethoxyethane), is built up of separate ion pairs with no significant interactions. The anion is formed from an Na atom O,S-chelated by two silanethiolate ligands of the same helicity (both P or both M), while the cation contains an Na atom solvated by two DME molecules. Because the structure is centrosymmetric, equal numbers of both conformational enantiomers are present in the crystal lattice.

Ammonium tri-tert-butoxy-silanethiol-ate.

The cations and anions of the title salt, NH(4) (+)·C(12)H(27)O(3)SSi(-), are linked by N-H⋯S and N-H⋯O hydrogen bonds into a linear chain that runs along the a axis of the monoclinic unit cell. The asymmetric unit contains two cations and two anions.

Bis(di-n-propyl-amine-κN)bis-(tri-tert-butoxy-silanethiol-ato-κS)chromium(II).

The title compound, [Cr(C(12)H(27)O(3)SSi)(2)(C(6)H(15)N)(2)], is a mol-ecular chromium(II) thiol-ate that is coordinated by two dipropyl-amine ligands in a square-planar environment. The mol-ecule lies on an inversion site.

Cubane-like structure of a silanethiol--primary amine assembly--a novel, unusual hydrogen bond pattern.

A reaction of silanethiol and primary amine leads to a product whose crystals are built of well-defined supermolecules--assemblies of four ammonium silanethiolate units (RS(-)H(3)N(+)R')(4) with a novel, unusual 3D hydrogen bond pattern.

The solvent-free thermal dehydration of hexitols on zeolites.

Dehydration of galactitol, D-glucitol and D-mannitol at high temperature in the presence of molecular sieves without solvent under an argon atmosphere is described. Cyclodehydration products with retention or inversion of the configuration at asymmetric carbon atoms, were observed. Reaction of galactitol yielded racemic 1,4-anhydrogalactitol in a first step and then racemic 1,4:3,6-dianhydroiditol. Complete analytical separations of exhaustively O-acetylated reaction products were achieved by GC and structures were assigned using co-injection with standards.

New class of quaternary ammonium salts, derivatives of methyl D-glucopyranosides.

Reactions of two aromatic and two aliphatic amines with methyl 6-O-p-toluenesulfonyl-alpha-D-glucopyranoside or methyl 6-O-p-toluenesulfonyl-beta-D-glucopyranoside were performed on a micro-scale. The synthesis and preparative isolation methods have been developed for quaternary N-(methyl 2,3,4-tri-O-acetyl-6-deoxy-alpha- and -beta-D-glucopyranoside-6-yl)ammonium salts derived from three amines: trimethylamine, 2-methylpyridine, and pyridine. The reaction products were examined with 1H, 13C NMR spectroscopy. N-(Methyl 2,3,4-tri-O-acetyl-6-deoxy-beta-d-glucopyranoside-6-yl)trimethylammonium tosylate was additionally analyzed with X-ray crystallography.

Synthesis and structure of selected quaternary N-(1,4-anhydro-5-deoxy-2,3-O-isopropylidene-D,L-ribitol-5-yl)ammonium salts.

The syntheses have been developed for quaternary N-(1,4-anhydro-5-deoxy-2,3-O-isopropylidene-D,L-ribitol-5-yl)ammonium salts derived from five aromatic amines, pyridine, 2-methylpyridine, 3-carbamoylpyridine, 4-(N,N-dimethylamino)pyridine, and quinoline, as well as two tertiary aliphatic amines, trimethylamine and triethylamine. Reactions of 1,4-anhydro-2,3-O-isopropylidene-5-O-tosyl-D,L-ribitol with tri-n-propylamine and tri-n-butylamine were unsuccessful. The products were identified on the basis of their 1H and 13C NMR spectra. The structure of N-(1,4-anhydro-5-deoxy-2,3-O-isopropylidene-D,L-ribitol-5-yl)trimethylammonium tosylate was additionally elucidated by X-ray diffractometry.

(2,2'-Bipyridine)bis(tri-tert-butoxysilanethiolato-kappaS)lead(II) and (4,7-diphenyl-1,10-phenanthroline-kappa2N,N')bis(tri-tert-butoxysilanethiolato-kappaS)lead(II) benzene hemisolvate.

In the title mononuclear lead silanethiolates, [Pb(C(12)H(27)O(3)SSi)(2)(C(10)H(8)N(2))], (I), and [Pb(C(12)H(27)O(3)SSi)(2)(C(24)H(16)N(2))].0.5C(6)H(6), (II), the Pb atom shows a distorted square-pyramidal coordination with a PbON(2)S(2) core in which one S atom lies in an axial position. Intermolecular pi-pi and C-H...pi interactions stabilize the structures. The benzene solvent molecule in (II) lies on an inversion centre.

The first compound with an unusual type of anion, [Li(SR)2]-: bis(mu2-aqua-d2)tetrakis(aqua-d2)dilithium(I) bis[bis(tri-tert-butoxysilanethiolato-kappa2O,S)lithate(I)] dihydrate-d2.

The title complex, [Li2(D2O)6][Li(C9H27SSiO3)2]2.2D2O, is the first compound with an S-M bond (M = alkali metal) within an unusual type of lithate anion, [Li(SR)2]- {where R is Si[OC(CH3)3]3}. There is a centre of symmetry located in the middle of the Li2O2 ring of the cation. All Li atoms are four-coordinate, with LiO4 (cations) and LiO2S2 (anions) cores. The singly charged [Li(SR)2]- anions are well separated from the doubly charged [Li2(D2O)6]2+ cations; the distance between Li atoms from differently charged ions is greater than 5 A. Both ion types are held within an extended network of O-D...O and O-D...S hydrogen bonds.

(Mu-tri-tert-butoxysilanethiolato)bis[(tetrahydrofuran)lithium(I)] and catena-poly[[bis(mu-tri-tert-butoxysilanethiolato)dilithium(I)]-mu-dimethoxyethane]: solvent coordination as the structure-forming factor.

The title compounds, mu-(tri-tert-butoxysilanethiolato-kappa2S:S)-bis[(tetrahydrofuran-kappaO)lithium(I)], [Li2(C12H27O3SSi)2(C4H8O)2], (I), and catena-poly[[bis(mu-tri-tert-butoxysilanethiolato)-1:2kappa(2)S;1kappaS:2kappaS,O-dilithium(I)]-mu-dimethoxyethane-kappa2O:O'], [Li2(C12H27O3SSi)2(C4H10O2)]n, (II), were obtained by the reaction of tri-tert-butoxysilanethiol with metallic lithium. The crude product, when recrystallized from tetrahydrofuran (THF) yields (I), and when recrystallized from 1,2-dimethoxyethane (DME) gives (II). Compound (I) forms centrosymmetric dimers in the solid state with an Li2S2 central core, whereas (II) forms infinitely long chains, in which the centrosymmetric dimeric units are linked together by the bidentate DME ligand (also residing on an inversion centre), thus forming a coordination polymer. The formation of a one-dimensional structure in (II) is a consequence of replacement of a monodentate THF solvent molecule with a bidentate DME molecule.