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Multinuclear ( 1 H, 13 C, 15 N, 19 F, 31 P) one‐ and two‐dimensional magnetic resonance study of tert ‐butylamino‐ tert ‐butyl‐fluorophosphane, tert ‐butylimino‐ tert ‐butylphosphane and of its dimer formed by [1 + 2] cycloaddition
Author(s) -
Wrackmeyer Bernd,
Köhler Christian
Publication year - 1993
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.1260310610
Subject(s) - chemistry , heteronuclear molecule , coupling constant , phosphorus 31 nmr spectroscopy , nmr spectra database , resonance (particle physics) , crystallography , nuclear magnetic resonance spectroscopy , carbon 13 , spectral line , dimer , analytical chemistry (journal) , nuclear magnetic resonance , stereochemistry , physics , atomic physics , nuclear physics , organic chemistry , particle physics , astronomy , chromatography
Multinuclear magnetic resonance studies ( 1 H, 13 C, 15 N, 31 P) of three phosphorus–nitrogen compounds [ tert ‐butylamino‐ tert ‐butylfluorophosphane (1), tert ‐butylimino‐ tert ‐butylphosphane (2) and its dimer (3)], in which numerous one‐ and two‐dimensional NMR experiments [heteronuclear shift correlations based on 1 J ( 13 C 1 H) or 1 J ( 15 N 1 H) and on long‐range coupling constants 2 J ( 13 C 1 H), 2 J ( 31 P 1 H), 3 J ( 15 N 1 H), 3 J ( 31 P 1 H) and 2D inverse 1 H/ 15 N correlations] were used, led to consistent assignment of the NMR spectra. By this means, incorrect data in the literature were corrected for 1 and 3 and new 15 N NMR data are reported, including isotope shifts 1 Δ 15/14 N( 31 P), obtained by 31 P INEPT–Hahn–echo extended (HEED) experiments. In the case of the monomeric iminophosphane 2, the largest negative value 1 Δ 15/14 N( 31 P) = −144 ppb was observed. Absolute signs of numerous coupling constants across one to five bonds were determined, involving the NMR active nuclei 1 H, 13 C, 15 N, 19 F and 31 P.