NMR Spectra and structures of organotin compounds

Petrosyan, V. S.

doi:10.1016/0079-6565(77)80005-8

Cited by 125 publications

(13 citation statements)

References 208 publications

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“…Analysis of the coupling constants and the H,H-COSY off-diagonal signals reveals correlation of the signal sets that belong to either the monomer or the dimer compound ( Figure 6). In the 13 C-NMR spectrum of 3 and 4, a 13 C 119 Sn coupling of 64.4 Hz (Figure 7) between the quaternary carbon and the tin center is observed, which is typical for a 2 J( 13 C 119 Sn) and which supports our description of 3 and 4 as an alcoholate derivative [32].…”

Section: Nmr Studies Of {Sn[oc(c 4 H 3 S) 3 ] 2 } 2 · 2 Toluene (2) supporting

confidence: 84%

Influence of the Solvent on the Formation of New Tin(II) Methoxides Containing Thienyl Substituents: Crystal Structure and NMR Investigations

Veith¹,

Belot²,

Hüch³

et al. 2009

Zeitschrift anorg allge chemie

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The synthesis, structural characterization, and NMR studies of new tin(II) alkoxides with thiophene-based substituents are presented. The reaction of ligand HOϪC(C 4 H 3 S) 3 (1) with bis(hexamethyldisilazyl)tin {Sn[N(SiMe 3 ) 2 ] 2 } in the ratio 2:1 in toluene yields the dinuclear compound {Sn[OC(C 4 H 3 S) 3 ] 2 } 2 · 2 toluene (2). The same reaction in tetrahydrofuran allows the isolation of two compounds: a dinuclear {Sn[OC(C 4 H 3 S) 3 ] 2 } 2 · 2 thf * Prof. Dr. M. VeithTo a solution of six equivalents of tris(2-thienyl)methanol (0.994 g, 3.33 mmol) in thf (20 mL) was added three equivalents of Sn[N(SiMe 3 ) 2 ] 2 (0.745 g, 1.69 mmol) in thf (5 mL). The mixture was stirred at room temperature for 2 days. The solution was concentrated, and colorless crystals were obtained at 5°C several days later (1.033 g) as a mixture of 3 and 4. M.p. 53Ϫ56°C (decomp.); 1 H NMR (400 MHz, CDCl 3 ), δ ϭ 7.3 (dd, 3 J H5,H4 ϭ 4.7 Hz and 4

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Section: Nmr Studies Of {Sn[oc(c 4 H 3 S) 3 ] 2 } 2 · 2 Toluene (2) supporting

confidence: 84%

Influence of the Solvent on the Formation of New Tin(II) Methoxides Containing Thienyl Substituents: Crystal Structure and NMR Investigations

Veith¹,

Belot²,

Hüch³

et al. 2009

Zeitschrift anorg allge chemie

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“…1 H NMR (400 MHz, CDCl 3 ) δ : 2.22 [8H, s, 2 J ( 119,117 Sn- 1 H) = 58.3 Hz, CH 2 ], 6.74 [8H, m, Ph], 7.01 [4H, m, Ph], 7.16 [8H, m, Ph]. 119 Sn{ 1 H} NMR (149 Hz, CDCl 3 ) δ : −37.1 (s); these values are consistent with those previously reported [ 22 ].…”

Section: Methodssupporting

confidence: 88%

Hydrogen activation using a novel tribenzyltin Lewis acid

Cooper¹,

Sapsford²,

Turnell-Ritson³

et al. 2017

Phil. Trans. R. Soc. A.

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Over the last decade there has been an explosion in the reactivity and applications of frustrated Lewis pair (FLP) chemistry. Despite this, the Lewis acids (LAs) in these transformations are often boranes, with heavier p-block elements receiving surprisingly little attention. The novel LA Bn3SnOTf (1) has been synthesized from simple, inexpensive starting materials and has been spectroscopically and structurally characterized. Subtle modulation of the electronics at the tin centre has led to an increase in its Lewis acidity in comparison with previously reported R3SnOTf LAs, and has facilitated low temperature hydrogen activation and imine hydrogenation. Deactivation pathways of the R3Sn+ LA core have also been investigated.This article is part of the themed issue ‘Frustrated Lewis pair chemistry’.

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“…Die aus der postulierten Pd±Cl´´´Sn-Koordination resultierende Pentakoordination des Zinnatoms Sn 2 wird durch die Hochfeldverschiebung seines 119 Sn-NMR-Signals bei 18.3 ppm im Vergleich zum Liganden 1 (d 119 Sn = 143) angezeigt. Der Strukturvorschlag fu È r 14 wird auch durch sein 1 H-NMR-Spektrum besta È tigt, das zwei intensita È tsgleiche Sn-Methylgruppensignale zeigt, wobei das fu È r Sn 1 bei ho È herem Feld (d = 0.27) mit einer Kopplungskonstanten 2 J(HC 119 Sn) von 47.8 Hz erscheint, wa È hrend jenes fu È r Sn 2 bei tieferem Feld (d = 0.59) liegt und entsprechend der Pentakoordination von Sn 2 eine ho È here 2 J(HC 119 Sn)-Kopplungskonstante von 67.1 Hz aufweist [22].…”

Section: Nickelkomplexe (3±8)unclassified

Ligandverhalten von P-funktionellen Organozinnhalogeniden: Nickel(II)-, Palladium(II)- und Platin(II)-halogenid-Komplexe mit Me2(Cl)SnCH2CH2PPh2

Baumeister

Hartung

Krug

et al. 2000

Z. anorg. allg. Chem.

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Inhaltsu È bersicht. Me 2 (Cl)SnCH 2 CH 2 PPh 2 (1) reagiert mit Nickel(II)-, Palladium(II)-und Platin(II)-halogeniden im Molverha È ltnis 2 : 1 zu den Komplexen [MX 2 {PPh 2 -CH 2 CH 2 Sn(Cl)Me 2 } 2 ] (M = Ni, Pd, Pt; X = Cl, Br) (3±6, 9, 10) (7, 8: M = Ni; Br anstelle von Cl). Von den Nickelkomplexen wurden jeweils das planare (3, 5, 7) und das tetraedrische (4, 6, 8) Isomer isoliert und charakterisiert. In Lo È sung liegen beide Isomere im Gleichgewicht vor. Die Kristallstrukturen und NMR-Daten belegen fu È r die planaren Nikkelkomplexe 3, 5, 7 sowie [MCl 2 {PPh 2 CH 2 CH 2 Sn(Cl)Me 2 } 2 ] (9: M = Pd; 10: M = Pt) die Existenz von intra-und intermolekularen M±Hal´´´Sn-Bru È cken. Im Ligand : Metall-Verha È ltnis 3 : 1 werden die Komplexe [M Å Cl{PPh 2 CH 2 -CH 2 Sn 7 Cl 2 Me 2 }{PPh 2 CH 2 CH 2 Sn(Cl)Me 2 } 2 ] (11: M = Pd; 12: M = Pt) gebildet, die als Zwitterionen vorliegen. Die Dehalogenierung von [PdCl 2 {PPh 2 CH 2 CH 2 Sn(Cl)Me 2 } 2 ] (9) mit Natriumamalgam bzw. Graphitkalium (C 8 K) fu È hrt zu den Palladacyclen cis-[Pd{PPh 2 CH 2 CH 2 SnMe 2 } 2 ] (13) und trans-[Pd(Cl)PPh 2 CH 2 CH 2 SnMe 2 {PPh 2 CH 2 CH 2 Sn(Cl)Me 2 }] (14). Von den Verbindungen 1, 3, 9, 11 und 12 wurden die Kristallstrukturen bestimmt. Sa È mtliche Verbindungen sind 1 H-, 31 P-und 119 Sn-NMR-spektroskopisch charakterisiert.Abstract. Me 2 (Cl)SnCH 2 CH 2 PPh 2 (1) reacts with Ni II , Pd II , and Pt II halides in molar ratio 2 : 1 forming the complexes [MX 2 {PPh 2 CH 2 CH 2 Sn(Cl)Me 2 } 2 ] (M = Ni, Pd, Pt; X = Cl, Br) (3±6, 9, 10) (7, 8: M = Ni; Br instead of Cl). The nickel complexes were isolated and characterized both as the planar (3, 5, 7) and the tetrahedral (4, 6, 8) isomer. Crystal structure analyses and NMR data indicate for the planar nikkel complexes 3, 5, 7 and [MCl 2 {PPh 2 CH 2 CH 2 Sn(Cl)Me 2 } 2 ] (9: M = Pd; 10: M = Pt) the existence of intra and intermolecular M±Hal´´´Sn bridges. In a ligand : metal molar ratio of 3 : 1 the complexes [M Å Cl{PPh 2 CH 2 CH 2 Sn 7 Cl 2 Me 2 }-{PPh 2 CH 2 CH 2 Sn(Cl)Me 2 } 2 ] (11: M = Pd; 12: M = Pt) are formed which represent intramolecular ion pairs. By dehalogenation of [PdCl 2 {PPh 2 CH 2 CH 2 Sn(Cl)Me 2 } 2 ] (9) with sodium amalgam and graphite potassium (C 8 K), respectively, the palladacycles cis-[Pd{PPh 2 CH 2 CH 2 SnMe 2 } 2 ] (13) and trans-[Pd(Cl)PPh 2 CH 2 CH 2 SnMe 2 {PPh 2 CH 2 CH 2 Sn(Cl)Me 2 }] (14) are formed. From the compounds 1, 3, 9, 11, and 12 the crystal structures are determined. All compounds are characterized by 1 H, 31 P, and 119 Sn NMR spectroscopy.

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NMR Spectra and structures of organotin compounds

Cited by 125 publications

References 208 publications

Influence of the Solvent on the Formation of New Tin(II) Methoxides Containing Thienyl Substituents: Crystal Structure and NMR Investigations

Influence of the Solvent on the Formation of New Tin(II) Methoxides Containing Thienyl Substituents: Crystal Structure and NMR Investigations

Hydrogen activation using a novel tribenzyltin Lewis acid

Ligandverhalten von P-funktionellen Organozinnhalogeniden: Nickel(II)-, Palladium(II)- und Platin(II)-halogenid-Komplexe mit Me2(Cl)SnCH2CH2PPh2

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