In:
Chemistry – A European Journal, Wiley, Vol. 9, No. 10 ( 2003-05-23), p. 2239-2244
Abstract:
The reaction of nido ‐[7,8,9‐PC 2 B 8 H 11 ] ( 1 ) with [{CpFe(CO) 2 } 2 ] (Cp=η 5 ‐C 5 H 5 − ) in benzene (reflux, 3 days) gave an η 1 ‐bonded complex [7‐Fp‐(η 1 ‐ nido ‐7,8,9,‐PC 2 B 8 H 10 )] ( 2; Fp=CpFe(CO) 2 ; yield 38 %). A similar reaction at elevated temperatures (xylene, reflux 24 h) gave the isomeric complex [7‐Fp‐(η 1 ‐ nido ‐7,9,10‐PC 2 B 8 H 10 )] ( 3 ; yield 28 %) together with the fully sandwiched complexes [1‐Cp‐ closo ‐1,2,4,5‐FePC 2 B 8 H 10 ] 4 a (yield 30 %) and [1‐Cp‐ closo ‐1,2,4,8‐FePC 2 B 8 H 10 ] 4 b (yield 5 %). Compounds 2 and 3 are isolable intermediates along the full η 5 ‐complexation pathway of the phosphadicarbaborane cage; their heating (xylene, reflux, 24 h) leads finally to the isolation of compounds 4 a (yields 46 and 52 %, respectively) and 4 b (yields 4 and 5 %, respectively). Moreover, compound 3 is isolated as a side product from the heating of 2 (yield 10 %). The structure of compound 4 a was determined by an Xray structural analysis and the constitution of all compounds is consistent with the results of mass spectrometry and IR spectroscopy. Multinuclear ( 1 H, 11 B, 31 P, and 13 C), two‐dimensional [ 11 B– 11 B]‐COSY, and 1 H{ 11 B(selective)} magnetic resonance measurements led to complete assignments of all resonances and are in excellent agreement with the structures proposed.
Type of Medium:
Online Resource
ISSN:
0947-6539
,
1521-3765
DOI:
10.1002/chem.200204704
Language:
English
Publisher:
Wiley
Publication Date:
2003
detail.hit.zdb_id:
1478547-X
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