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Fig. 3. Newman projection of (2).
3.2. Synthesis of (2)
Sodium (0.13 g; 5.8 mmol) was added to a stirred
suspension of (1) (2.81 g; 5.8 mmol) in ammonia (50
ml) at −70°C. After 4 h stirring at this temperature
ammonia was evaporated at 0°C, the solid was dried in
vacuo at r.t., n-hexane (80 ml) was added to the solid
and stirred for 30 min: insoluble residues were filtered.
After filtration of the yellow liquid solvent was re-
moved in vacuo at 0°C until the first crystals appeared.
Cooling the concentrated solution to −30°C for 30 h
affords yellow and green crystals which were separated
and dried in vacuo. The yellow and green crystals were
characterized as an identical product (2). Yield: 2.50 g;
1.6 mmol of 2, 56%. Melting point: 194°C.
Found: C, 47.83; H, 4.90. C36H44Bi2O calc.: C, 47.48;
H, 4.87. 1H-NMR (THF-d8): l (ppm): 2.44, s, 12H,
o-CH3, 2.48, s, 6H, p-CH3, 7.25, s, 4H, C6H2; 13C-
NMR: l (ppm): 20.60, CH3, 22.97, CH3, 130.44,
130.67, 136.66, 145.01, aromatic carbons. EI-MS (70
eV): m/z, ion, intensity %: 791, M-C6H2(CH3)3, 14.2;
537, Bi2[C6H2(CH3)3], 1 2; 565, Bi[C6H2(CH3)3]3–H,
3.9; 463, [C6H2(CH3)3BiO, 4.1; 447, Bi[C6H2(CH3)3]2,
100.0; 418, Bi2, 1.0; 342, C6H2(CH3)3BiO+H, 3.4; 327,
BiC6H2(CH3)3, 60.1; 209, Bi, 71.0; 119, C6H2(CH3)3,
39.3. IR (Nujol, w cm−1): 149 m/br, 174 vst, 200 vst,
329 m, 382 m, 391 m, 473 m, 493 m, 545 vw, 607 w, 698
vw, 845 vw, 1025 vw, 1157 vw/br, 1287 vw, 1553 vw,
1593 vw, 2726 vw/br, 3443 w/br.
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[29] S.-H. Shin, PhD Thesis, University of Marburg, Marburg, Ger-
many, 1989.
[30] X.-W. Li, PhD Thesis, Marburg University, Marburg, Germany,
1994.
Acknowledgements
This work was supported by DFG through a grant
for X.-W. Li within the framework of the
‘Graduiertenkolleg Metallorganische Chemie’ at the
Philipps-Universita¨t Marburg. Support from the ‘Fonds
der Chemischen Industrie, VCI’ for J.L. and W.M. is
gratefully acknowledged.
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.
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