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1,1′‐Bis(stannyl)‐ and 1,1′‐Bis(chlorostannyl)ferrocenes Studied by Multinuclear Magnetic Resonance, Temperature‐Dependent 57 Fe‐ and 119 Sn‐Mössbauer Spectroscopy, and Electrochemistry
Author(s) -
Herberhold Max,
Milius Wolfgang,
Steffl Udo,
Vitzithum Klaus,
Wrackmeyer Bernd,
Herber Rolfe H.,
Fontani Marco,
Zanello Piero
Publication year - 1999
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/(sici)1099-0682(199901)1999:1<145::aid-ejic145>3.0.co;2-x
Subject(s) - chemistry , ferrocene , mössbauer spectroscopy , electrochemistry , nuclear magnetic resonance spectroscopy , spectroscopy , crystallography , intermolecular force , molecule , stereochemistry , organic chemistry , electrode , physics , quantum mechanics
The 1,1′‐bis(chlorostannyl)‐substituted ferrocenes Fe(C 5 H 4 –SnMe 2 Cl) 2 ( 2 ), Fe(C 5 H 4 –SnMeCl 2 ) 2 ( 3 ) and Fe(C 5 H 4 –SnCl 3 ) 2 ( 4 ) were prepared, starting from 1,1′‐bis(trimethylstannyl)ferrocene ( 1 ). Treatment of the chlorides with Li[AlH 4 ] afforded the 1,1′‐bis(hydridostannyl)‐subsituted ferrocenes Fe(C 5 H 4 –SnMe 2 H) 2 ( 5 ), Fe(C 5 H 4 –SnMeH 2 ) 2 ( 6 ) and Fe(C 5 H 4 ‐SnH 3 ) 2 ( 7 ), respectively. All complexes 1 – 7 were studied by 1 H‐, 13 C‐, and 119 Sn‐NMR spectroscopy with 1D and 2D techniques. The compounds 1 – 4 were investigated by temperature‐dependent 119 Sn‐ and 57 Fe‐Mössbauer spectroscopy. The electrochemistry of 1 – 5 gave evidence of reversible one‐electron oxidation processes. The molecular structure of 1,1′‐bis(trichlorostannyl)ferrocene ( 4 ) was determined by X‐ray structural analysis, and there was no indication of intra‐ or intermolecular Sn ··· Cl ··· Sn interactions. This direct structural information proved to be consistent with both the Mössbauer and the solution NMR spectroscopic data.