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Trimethylstannylboranes—inverse detection of broad 119 Sn NMR signals in solution and solid‐state 119 Sn cross‐polarization magic angle spinning NMR
Author(s) -
Wrackmeyer Bernd,
Kupče Ēriks,
Kümmerlen Jörg
Publication year - 1992
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.1260300509
Subject(s) - chemistry , borane , nmr spectra database , magic angle spinning , spectral line , j coupling , crystallography , analytical chemistry (journal) , solid state nuclear magnetic resonance , nuclear magnetic resonance spectroscopy , stereochemistry , nuclear magnetic resonance , organic chemistry , physics , astronomy , catalysis
Extremely broad 119 Sn resonances, as the result of 1 J ( 119 Sn, 11 B) scalar coupling, were readily detected, even for diluted samples (5 mg in 0.5 ml of C 6 D 6 ), via inverse two‐dimensional 1 H{ 119 Sn} NMR experiments. Two bis(amino)trimethylstannylboranes and four dialkylaminobis(trimethylstannyl)boranes were studied. The reaction between diisopropylaminobis(trimethylstannyl)borane and trimethoxyborane was monitored by the same technique, leading to the detection of diisopropylaminomethoxytrimethylstannylborane and dimethoxytrimethylstannylborane as reaction products. Crystalline dicyclohexylaminobis(trimethylstannyl)borane was studied by 119 Sn CP/MAS NMR. In spite of the proximity of 119 Sn to the quadrupolar 11 B nucleus, meaningful spectra could be obtained in a short time (≤ 2 h).