α,ω-Bis(trichlorostannyl)alkanes: unravelling the hydrolysis pathway to organotin-oxo oligomers

New α,ω-bis(trichlorostannyl)alkanes, Cl₃Sn(CH₂)_nSnCl₃ [n = 3-5, 8], have been synthesized via tin-phenyl bond cleavage reactions on α,ω-bis(triphenylstannyl)alkanes, Ph₃Sn(CH₂)_nSnPh₃ [n = 3-5, 8], using either SnCl₄ or concentrated hydrochloric acid. Some key missing links, (H₂O)Cl₃Sn(CH₂)₃SnCl₃(H₂O) (1a) and (H₂O)₂Cl₃Sn(CH₂)₃SnCl₃(H₂O)₂ (6), in the hydrolysis pathway of organotin trichlorides were identified. Crystal structures of the nonassociated di-tin compounds (H₂O)Cl₃Sn(CH₂)₃SnCl₃(H₂O) (1a) and (H₂O)₂Cl₃Sn(CH₂)₃SnCl₃(H₂O)₂ (6, isolated as the 18-crown-6 cocrystal acetonitrile solvate) as well as the polymeric hydrolysis product [H₂O(OH)Cl₂Sn(CH₂)₃SnCl₂(OH)H₂O·₂H2O]_n (7·2H₂O) are reported.

α,ω-Bis(trichlorostannyl)alkanes as Bis(monodentate) lewis acids toward halide ions

The reactions between X₃Sn(CH₂)_nSnX₃ (X = Cl, Br; _n = 1, 3, 4, 8) and halide in solution are described. ¹¹⁹Sn NMR spectroscopy (CD₂Cl₂) indicates formation of five-coordinate dinuclear 1:2 adducts, [X₄Sn(CH₂)_nSnX₄]^2-, with chloride and bromide. A trigonal-bipyramidal geometry has been confirmed in the solid state for the compound having X = Cl and _n = 4. In contrast, fluoride reacts with X₃Sn(CH₂)_nSnX₃ to give six-coordinate tin species, [F₅Sn(CH₂)_nSnF₅].^4- There was no evidence indicating that the tin atoms could act as a bidentate acid.

Synthesis and preliminary analytical evaluation of the chemiluminescence from (4-[4-(dichloromethylsilanyl)-butyl]-4`-methyl-2,2`-bipyridyl)bis(2,2`-bipyridyl)ruthenium(II) covalently bonded to silica particles

This paper describes, for the first time, a simple and effective synthetic route for covalently bonding the chemiluminescence reagent, (4-[4-(dichloromethylsilanyl)-butyl]-4’-methyl-2,2’-bipyridyl)bis(2,2’-bipyridyl)ruthenium(II) onto silica particles. The subsequent preparation of chemically regeneratable detection cells and their preliminary analytical evaluation with both sequential injection analysis and flow injection analysis are also reported. Unoptimised analytical figures of merit were established for standard solutions of codeine and sodium oxalate with detection limits calculated from three times the standard deviation of the blank signal, of 1 × 10^–8 M and 3 × 10^–7 M respectively. The chemically immobilised reagent exhibited some intriguing solvent and kinetic effects, which are also briefly discussed.

Synthesis and structure of bis(para-methoxyphenyl)selenoxide and its monohydrate. theoretical considerations of the hydration of diorganoselenium oxides

The title compound was prepared by base hydrolysis of (p-MeOC₆H₄)₂SeCl₂ in water and isolated as the crystalline monohydrate, (p-MeOC₆H₄)₂SeO·H₂O, in which the water molecule is associated via hydrogen-bonding. Water-free (p-MeOC₆H₄)₂SeO was obtained crystalline after drying and recrystallisation from toluene. Both crystal phases were investigated by single crystal X-ray diffraction. Preliminary DFT calculations at the B3LYP/LANL2DZdp level of theory suggest that the hydrogen bonded complexes R₂SeO·H₂O (R = H, Me, Ph) are by 2.79, 3.36 and 11.10 kcal mol^-1 more stable than the corresponding elusive diorganoselenium dihydroxides R₂Se(OH)₂. The hydrogen bond energies of R₂SeO·H₂O (R = H, Me, Ph) are 5.98, 7.18 and 5.89 kcal mol^-1.

catena-Poly[[[bis[(-)-O-bornyldithiocarbonato-κ2S,S']nickel(II)]-μ-4,4'-bipyridine-κ2N:N'] chloroform disolvate]

The Ni atom in the linear polymeric title complex, {[Ni(C₁₁H₁₇OS₂)₂(C₁₀H₈N₂)]·2CHC1₃}_n or {Ni[S₂C(-)-OC₁₀H₁₇)]₂(NC₅H₄C₅H₄N)·2CHC1₃}_n, is octahedrally coordinated within a trans-N₂S₄ donor set. There are two crystallographically independent polymers and two independent CHC1₃ molecules in the structure. For each polymer unit, the Ni atom and the axis of the 4,4'-bipyridine ligand are located on a twofold axis.

Synthesis and polymerisation of α,ω-bis(3-pyrrolyl)alkanes

The synthesis, characterisation and polymerisation studies of a homologous series of α,ω-bis(pyrrolyl)alkanes are described. These α,ω-bis(pyrrolyl)alkanes were produced using Friedel–Crafts acylation followed by reduction of the carbonyl group using Red-Al®. Chemical polymerisation of the resultant dimers using FeCl₃ produced poly(α,ω-bis(pyrrolyl)alkane) films, which were characterised by SEM, FTIR and tested for conductivity.

Conductive poly(α,ω-bis(3-pyrrolyl)alkanes)-coated wool fabrics

Cross-linked poly(α,ω-bis(3-pyrrolyl)alkanes) were directly applied to woven wool substrates by either chemical, vapour or mist polymerization methods. Choice of dopant could greatly improve the surface resistance. The optimum coating on textiles with the lowest surface resistance, highest colour-fastness and stability was achieved using a mist polymerization method with 1,8-bis(pyrrolyl)octane, iron(III) chloride (FeCl₃) as the oxidant and p-toluene sulfonic acid sodium salt (pTSA) as the dopant.