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Balova, Irina A.
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article
Reactions of diacetylene ligands with trinuclear clusters. 3. Cyclization of diynes with β-amino moieties on the metal core of [H2Os3(CO)10]
Abstract
<p>Reactions of [H<sub>2</sub>Os<sub>3</sub>(CO)<sub>10</sub>] with the substituted diynes R-C<sub>2</sub>-C<sub>2</sub>-R′ (1, R = Ph, R′ = CH<sub>2</sub>NHPh; 2, R = Ph, R′ = CH<sub>2</sub>NHCH<sub>2</sub>Ph; 3, R = R′ = CH<sub>2</sub>NHPh) afford the clusters [HOs<sub>3</sub>(CO)<sub>10</sub>(L)] (L = {μ-η<sup>1</sup>:η<sup>2</sup>-PhCH<sub>2</sub>C(H)=C-C(H)=C-NPh} (4), {μ-η<sup>1</sup>:η<sup>2</sup>-PhCH<sub>2</sub>C(H)=C-C(H)= C-NCH<sub>2</sub>Ph} (5), and {μ-η<sup>1</sup>:η<sup>1</sup>-CH<sub>3</sub>CC=C-C(H)=C(H)-NPh} (6), which have been characterized by single-crystal X-ray diffraction analyses as well as by various spectroscopic methods. In clusters 4-6, the starting diynes 1-3 have been rearranged to form substituted pyrrolyl rings which bridge two osmium atoms in η<sup>1</sup>:η<sup>2</sup>- (4, 5) or η<sup>1</sup>:η<sup>1</sup>- (6) coordination modes depending on the nature of substituents in 1-3. A possible reaction pathway for the diyne cyclization reactions that yield 4-6 involves initial transfer of a hydride onto a coordinated diyne followed by a series of 1,3-shifts and subsequent nucleophilic attack of the nitrogen on the third carbon atom of the diyne system to afford the five-membered pyrrolyl ring. Cluster 6 and its previously characterized furanyl analogue [HOs<sub>3</sub>(CO)<sub>10</sub>{μ-η<sup>1</sup>:η<sup>1</sup>-(OCH- CHCC)-C-CH<sub>3</sub>)}] (7) undergo facile thermal transformation accompanied by the loss of a CO ligand to give the clusters [HOs<sub>3</sub>(CO)<sub>9</sub>{μ<sub>3</sub>,η<sup>3</sup>- CH<sub>3</sub>CC=C-C(H)=C(H)-NPh}] (8) and [HOs<sub>3</sub>(CO)<sub>9</sub>{μ<sub>3</sub>,η<sup>3</sup>-(OCH=CHC= CCCH<sub>3</sub>)}] (9). In both 8 and 9, single-crystal X-ray analysis revealed the presence of pentagonal pyramid cluster cores containing three osmium and three carbon atoms.</p>