Organoborierung von Tetrakis(trimethylsilylethinyl)stannan – Röntgenstrukturanalyse eines 5‐Stannaspiro[4.4]nona‐1,3,6,8‐tetraen‐Derivates[1]
- 1 March 1992
- journal article
- research article
- Published by Wiley in European Journal of Inorganic Chemistry
- Vol. 125 (3) , 643-650
- https://doi.org/10.1002/cber.19921250316
Abstract
Organoboration of Tetrakis(trimethylsilylethynyl)stannane – X‐ray Structure of a 5‐Stannaspiro[4.4]nona‐1,3,6,8‐tetraene DerivativeTetrakis(trimethylsilylethynyl)stannane (1) reacts with non‐cyclic trialkylboranes BR3 [2, R = Me (a), Et (b), Pr (c), iPr (d)] and 9‐alkyl‐9‐borabicyclo[3.3.1]nonanes[2e (alkyl = Et), 2f (alkyl = neopentyl)] to give the 3,8‐dialkyl‐2,7‐bis(dialkylboryl)‐1,4,6,9‐tetrakis(trimethylsilyl)‐5‐stannaspiro[4.4]nona‐1,3,6,8‐tetraenes 5a to f in high yield. The reaction proceeds stepwise, and intermediates as well as final products were characterized by 1H, 11B, 13C, 29Si, 119Sn NMR spectroscopy. According to an X‐ray structure analysis of 5f · 0.5 CH2Cl2 (space group P2/c) the endocyclic CSnC bond angles are small [84.9(2) and 84.2(2)°] and the two five‐membered rings are not exactly planar. Steric crowding causes a strong twist of the skeleton of the other ring systems. The agreement between solid‐state and liquid‐phase NMR data shows that main structural features are retained in solution.Keywords
This publication has 45 references indexed in Scilit:
- Trimethylsilyl-, trimethylstannyl- and trimethylplumbylmethane derivatives studied by one- and two-dimensional multinuclear magnetic resonance—sign iSpectrochimica Acta Part A: Molecular Spectroscopy, 1991
- Application of INEPT to 13C NMR of alkynylmetal compounds and the convenient sign determination of coupling constants and by two-dimensional 13C/1H heteronuclear shift correlationJournal of Magnetic Resonance (1969), 1990
- Silylmethyl and silylamino groups as ligands in tin(II), tin(IV), lead(II) and lead(IV) compounds—a multinuclear magnetic resonance studySpectrochimica Acta Part A: Molecular Spectroscopy, 1990
- A Sensitive Multichannel Detection System for Surface Raman SpectroscopyApplied Spectroscopy, 1988
- Carbon-13 and tin-119 relaxation studies of some axially symmetrical organotin compoundsJournal of Magnetic Resonance (1969), 1988
- Observation of 13C13C couplings with enhanced sensitivityJournal of Magnetic Resonance (1969), 1982
- Indirect measurement of proton relaxation rates by “INEPT” polarization transfer to carbon-13: Proton spin-lattice relaxation in cholesteryl acetate solutionsJournal of Magnetic Resonance (1969), 1980
- NMR Spectra and structures of organotin compoundsProgress in Nuclear Magnetic Resonance Spectroscopy, 1977
- Studies in Stereochemistry. V. The Effect of F-Strain on the Relative Base Strengths of Ammonia and Trimethylamine1Journal of the American Chemical Society, 1945
- Experimentelle Beiträge zum Valenz‐Problem des Bors, VI.: Die Valenz‐Äußerungen des Bors im Tri‐ p ‐anisyl‐, tri‐ tert .‐butyl‐ und Tri‐ sek. ‐propyl‐bor, sowie Versuche über die Existenzfähigkeit gemischter TrialkylborverbindungenBerichte der deutschen chemischen Gesellschaft (A and B Series), 1931