A useful procedure for the preparation of chemically synthesized and cross-linked polydimethylsiloxane (PDMS) gels is presented, which does not require β-irradiation for cross-linking. NMR spectra of high quality are obtained, such that even mixtures of compounds exhibiting similar NMR spectra like interconverting stereoisomers can be investigated in the residual dipolar coupling (RDC) approach of organic structure determination.
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