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Synthesis of Trithia-Borinane Complexes Stabilized in Diruthenium Core: [(Cp*Ru)<sub>2</sub>(η<sup>1</sup>-S)(η<sup>1</sup>-CS){(CH<sub>2</sub>)<sub>2</sub>S<sub>3</sub>BR}] (R = H or SMe)
oleh: Koushik Saha, Urminder Kaur, Rosmita Borthakur, Sundargopal Ghosh
Format: | Article |
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Diterbitkan: | MDPI AG 2019-02-01 |
Deskripsi
The thermolysis of <i>arachno</i>-<b>1</b> [(Cp*Ru)<sub>2</sub>(B<sub>3</sub>H<sub>8</sub>)(CS<sub>2</sub>H)] in the presence of tellurium powder yielded a series of ruthenium trithia-borinane complexes: [(Cp*Ru)<sub>2</sub>(η<sup>1</sup>-S)(η<sup>1</sup>-CS){(CH<sub>2</sub>)<sub>2</sub>S<sub>3</sub>BH}] <b>2</b>, [(Cp*Ru)<sub>2</sub>(η<sup>1</sup>-S)(η<sup>1</sup>-CS){(CH<sub>2</sub>)<sub>2</sub>S<sub>3</sub>B(SMe)}] <b>3</b>, and [(Cp*Ru)<sub>2</sub>(η<sup>1</sup>-S)(η<sup>1</sup>-CS){(CH<sub>2</sub>)<sub>2</sub>S<sub>3</sub>BH}] <b>4</b>. Compounds <b>2</b>⁻<b>4</b> were considered as ruthenium trithia-borinane complexes, where the central six-membered ring {C<sub>2</sub>BS<sub>3</sub>} adopted a boat conformation. Compounds <b>2</b>⁻<b>4</b> were similar to our recently reported ruthenium diborinane complex [(Cp*Ru){(η<sup>2</sup>-SCHS)CH<sub>2</sub>S<sub>2</sub>(BH<sub>2</sub>)<sub>2</sub>}]. Unlike diborinane, where the central six-membered ring {CB<sub>2</sub>S<sub>3</sub>} adopted a chair conformation, compounds <b>2</b>⁻<b>4</b> adopted a boat conformation. In an attempt to convert <i>arachno</i>-<b>1</b> into a <i>closo</i> or <i>nido</i> cluster, we pyrolyzed it in toluene. Interestingly, the reaction led to the isolation of a capped butterfly cluster, [(Cp*Ru)<sub>2</sub>(B<sub>3</sub>H<sub>5</sub>)(CS<sub>2</sub>H<sub>2</sub>)] <b>5</b>. All the compounds were characterized by <sup>1</sup>H, <sup>11</sup>B{<sup>1</sup>H}, and <sup>13</sup>C{<sup>1</sup>H} NMR spectroscopy and mass spectrometry. The molecular structures of complexes <b>2</b>, <b>3</b>, and <b>5</b> were also determined by single-crystal X-ray diffraction analysis.