Preparation and spectroscopic studies of dialkyltin hydroxide nitrate, trimethyltin nitrate and its monohydrate

Yasuda, Kiyoshi; Okawara, Rokuro

doi:10.1016/s0022-328x(00)82738-2

Cited by 32 publications

(5 citation statements)

References 9 publications

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“…The speciation of cationic dialkyltin(IV) compounds in strongly polar solvents, such as water and acetonitrile, has attracted appreciable interest over the past 50 years. − In aqueous solution, dialkyltin dichlorides, R 2 SnCl 2 (R = Me, Et, Bu), dissociate into hydrated dialkyltin dications, [R 2 Sn(H 2 O) 4 ] 2+ , and chloride anions . Solvated dialkyltin dications, [R 2 SnL 4 ] 2+ (L = H 2 O, MeCN), are also formed upon addition of strong acids HX, such as HNO 3 , HClO 4 , and HO 3 SCF 3 , to suspensions of dialkyltin oxides, R 2 SnO, in polar solvents such as water and acetonitrile. − When solutions containing solvated dialkyl dications [R 2 SnL 4 ] 2+ are slowly evaporated under air, the nature of the deposited diorganotin products strongly depends on the identity and concentration of the counterions. Dialkyltin dichlorides, R 2 SnCl 2 , are obtained at high concentrations of chloride ions, whereas in the presence of weakly coordinating oxygen anions partly hydrolyzed dialkyltin−oxo species, such as [R 2 Sn(OH)X] 2 10-14,16,18 ,, (X = NO 3 - , ClO 4 - , O 3 SCF 3 - ) ( A ) and [R 2 (X)SnOSn(Y)R 2 ] 2 11,16,17 (X, Y = OH - , NO 3 - , ClO 4 - , O 3 SCF 3 - ) ( B ), are dominant (Chart ).…”

Section: Introductionmentioning

confidence: 99%

Hydrolysis of Dinuclear Spacer-Bridged Diorganotin(IV) Triflates. A Novel Cationic Double Ladder with Supramolecular Association

et al. 2003

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A series of oligomethylene-bridged diorganotin triflates R(OTf)2Sn(CH2) n Sn(OTf)2R (R = CH2SiMe3; n = 3, 4, 8, 10) were synthesized by reaction of triflic acid with the precursor oxides R(O)Sn(CH2) n Sn(O)R. On the basis of 119Sn NMR (in acetonitrile) the triflates appear to be the simple six-coordinated ionic species [(MeCN)4(RSn(CH2) n SnR)(MeCN)4]2+. These triflates readily undergo hydrolysis to give products, the identity of which depends on the length of the oligomethylene bridge. For n = 3 (5), the solid-state structure shows association of two dimeric units, which results in a tetracationic double ladder. Extensive hydrogen bonding gives rise to a supramolecular association. Solution 119Sn NMR and ES MS suggest some dissociation of 5 into dimers containing four tin atoms and possibly monomers containing two tin atoms. A rudimentary solid-state structure for n = 4 (6) indicates a linear polymer based on dimeric (four tin atoms) units. The structure of 6 also features extensive hydrogen bonding, this time effectively giving rise to alternating layers of cations and anions.

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Section: Introductionmentioning

confidence: 99%

Hydrolysis of Dinuclear Spacer-Bridged Diorganotin(IV) Triflates. A Novel Cationic Double Ladder with Supramolecular Association

et al. 2003

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“…3£/(l + 9|2) (7) where = ( 8 8")/[ 8 7 A< 1 Asn-p3> -78 _ /3]. In Table 1, it is shown that this ratio equal 0.14 ± 0.03.…”

Section: Resultsmentioning

confidence: 87%

NMR Study of the Solution-State Dynamics and Solid-State Structure of Tri-n-butyltin Fluoride

Kim¹,

Labouriau²,

Taylor³

et al. 1994

J. Phys. Chem.

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Dynamics and structure of tri-n-butyltin fluoride in n-hexane solutions were probed using (tin-1 19) nuclear magnetic resonance spin relaxation methodologies. Significant relaxation-induced polarization transfer effects were observed and exploited. The experimental observations indicate that the tri-n-butyl fluoride exists in a polymeric form in solution. For a 0.10% (w/w) solution at 25 OC, NMR reveals significant orientational/ exchange relaxation on both the microsecond and nanosecond time scales. Solution-state and solid-state parameters are compared and contrasted.

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“…Similar results were formerly obtained by Yasuda and Okawara. 31 While the structure of 1a did not depend on the reaction conditions applied, those of 1b differed depending on the molar ratio of oxide to acid. In the following, we will label these two modifications ␣-1b and ␤-1b.…”

Section: Methodsmentioning

confidence: 90%

“…6.3687 (6) 8.5583 (3) 6.2598 (3) 7.4015(4) 6.4907 (2) 17.7506 (7) 21.4592 (3) 14.8248(4) b (Å) 6.4171 (6) 12.9680 (5) 8.7798 (4) 13.1003 (6) 14.5595 (7) 10.3148 (3) 9.9849 (2) 10.0441(4) c (Å) 8.6940 (9) 18.2039 (7) 8.8163 (4) 31 …”

Section: Me 2 Sn(no 3 )(Oh) 1aunclassified

Reaction products of diorganotin(IV) oxides, R₂SnO, with nitric acid. Part 1: R = methyl, ethyl, and isopropyl

ReuterHans

ReicheltMartin

2014

Can. J. Chem.

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The reaction of diorganotin(IV) oxides, R 2 SnO with R = Me, Et, and i-Pr, with nitric acid in different stoichiometric ratios resulted in the formation of different products depending on the organic groups. The diorganotin(IV) nitrate hydroxides Me 2 Sn(NO 3 )(OH) (1a) Et 2 Sn(NO 3 )(OH), ␣-1b, ␤-1b, i-Pr 2 Sn(NO 3 )(OH) (1c), the diisopropyltin(IV) dinitrate dihydrate, i-Pr 2 Sn(NO 3 ) 2 ·2H 2 O (2c) and the diisopropyltin(IV) nitrate oxalate dihydrate, [i-Pr 2 Sn(NO 3 )] 2 Ox·2H 2 O (3) as side-product. On examination of the solubility of the primary reaction products in different solvents, the two additional compounds Me 2 Sn(NO 3 )(OH)·DMSO (4) and 2i-Pr 2 Sn(NO 3 ) 2 ·3DMSO = [i-Pr 2 Sn(NO 3 )(dmso) 3 ] [i-Pr 2 Sn(NO 3 ) 3 ] (5) have been isolated. All compounds have been structurally characterized by single crystal X-ray diffraction with special respect to dimensionality (1a, ␣-1b, 1c = dimeric molecules hydrogen bonded to one-dimensional chains; ␤-1b = two-dimensional coordination polymer; 2c = monomeric; 3 = monomeric, tin atoms linked via a double side-on chelating oxalate ion; 4 = dimeric, 5 = monomeric anion/cation), tin coordination (trigonalbipyramidal = 1a, ␣-1b, 1c; six-fold = ␤-1b; seven-fold = 3, 4, 5-cation; eight-fold = 2c, 5-anion) and nitrate bonding modes (monodentate = 1a, ␣-1b, 1c; unsymmetrical bidentate = 3, symmetrical bidentate = 3, 4, 5-cation, 5-anion; syn-anti bridging = ␤-1b), the latter one being analysed using both, Sn-O and N-O distances.Résumé : La réaction des oxydes de diorganoétain(IV) oxides, R 2 SnO (où R=Me, Et et i-Pr), avec l'acide numériques dans diverses proportions stoechiométriques a conduit à la formation de différents produits dont la nature dépendait des groupes organiques : les hydroxydes nitrate de diorganoétain(IV), de formules Me 2 Sn(NO 3 )(OH) (1a), Et 2 Sn(NO 3 )(OH) (á-1b et â-1b) et i-Pr 2 Sn(NO 3 )(OH) (1c), le dinitrate de diisopropylétain(IV) dihydraté, i-Pr 2 Sn(NO 3 ) 2 ·2H 2 O (2c), et un sous-produit, l'oxalate nitrate de diisopropylétain(IV) dihydraté, [i-Pr 2 Sn(NO 3 )] 2 Ox·2H 2 O (3). Après examen de la solubilité des produits primaires de réaction dans différents solvants, deux autres composés ont été isolés : Me 2 Sn(NO 3 )(OH)·DMSO (4) et 2i-Pr 2 Sn(NO 3 ) 2 ·3DMSO = [i-Pr 2 Sn(NO 3 )(dmso) 3 ] [i-Pr 2 Sn(NO 3 ) 3 ] (5). La structure de ces composés a été déterminée par cristallographie aux rayons X, en particulier la dimensionnalité (1a, á-1b, 1c = molécules dimériques reliées par liaisons hydrogène à des chaînes unidimensionnelles; â-1b = polymère de coordination bidimensionnel; 2c = monomère; 3 = monomère; atomes d'étain reliés par l'intermédiaire d'un ion double latéral d'oxalate chélateur; 4 = dimère, 5 = anion ou cation monomérique), coordination de l'étain (trigonale-bipyramidale, avec 1a, á-1b, 1c; à six plis, avec â-1b; à sept plis, avec 3, 4 et le cation 5; à huit plis, avec 2c et l'anion 5) et les modes de liaisons du nitrate (monodentate, avec 1a, á-1b et 1c; bidentate asymétrique, avec 3, bidentate symétrique, avec 3, 4, le ca...

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Preparation and spectroscopic studies of dialkyltin hydroxide nitrate, trimethyltin nitrate and its monohydrate

Cited by 32 publications

References 9 publications

Hydrolysis of Dinuclear Spacer-Bridged Diorganotin(IV) Triflates. A Novel Cationic Double Ladder with Supramolecular Association

Hydrolysis of Dinuclear Spacer-Bridged Diorganotin(IV) Triflates. A Novel Cationic Double Ladder with Supramolecular Association

NMR Study of the Solution-State Dynamics and Solid-State Structure of Tri-n-butyltin Fluoride

Reaction products of diorganotin(IV) oxides, R₂SnO, with nitric acid. Part 1: R = methyl, ethyl, and isopropyl

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Preparation and spectroscopic studies of dialkyltin hydroxide nitrate, trimethyltin nitrate and its monohydrate

Cited by 32 publications

References 9 publications

Hydrolysis of Dinuclear Spacer-Bridged Diorganotin(IV) Triflates. A Novel Cationic Double Ladder with Supramolecular Association

Hydrolysis of Dinuclear Spacer-Bridged Diorganotin(IV) Triflates. A Novel Cationic Double Ladder with Supramolecular Association

NMR Study of the Solution-State Dynamics and Solid-State Structure of Tri-n-butyltin Fluoride

Reaction products of diorganotin(IV) oxides, R2SnO, with nitric acid. Part 1: R = methyl, ethyl, and isopropyl

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Reaction products of diorganotin(IV) oxides, R₂SnO, with nitric acid. Part 1: R = methyl, ethyl, and isopropyl