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Abstract <p>The reaction of the dinuclear precursor [(<i>p</i>‑cymene)RuCl<sub>2</sub>]<sub>2</sub> with <i>ortho</i>‑carborane, elemental sulfur and 1,1‑diphenyl‑2‑propyn‑1‑ol (HC≡CC(OH)Ph<sub>2</sub>) yields two carborane‑incorporating ruthenium complexes <i>via</i> divergent pathways. Besides the known B–H activation product (<i>p</i>‑cymene)Ru[H<sub>9</sub>B<sub>10</sub>C<sub>2</sub>S<sub>2</sub>CH<sub>2</sub>CC(OH)Ph<sub>2</sub>] (<b>2</b>), a novel complex (<i>p</i>‑cymene)Ru(H<sub>10</sub>B<sub>9</sub>C<sub>2</sub>S<sub>2</sub>CHCCPh<sub>2</sub>) (<b>1</b>) was isolated and fully characterized. Its formation proceeds through initial dehydration of the alkynol to give an allenylidene intermediate, followed by attack of two sulfur atoms at the C=C=CPh<sub>2</sub> unit and concomitant extrusion of one boron atom from the <i>closo</i>‑C<sub>2</sub>B<sub>10</sub>H<sub>10</sub> cage, resulting in a rare <i>nido</i>‑C<sub>2</sub>B<sub>9</sub> metallacyclic framework. Complex <b>1</b> was characterized by IR, NMR, MS, elemental analysis, and single‑crystal X‑ray diffraction. It crystallizes in the monoclinic space group <i>P</i>2<sub>1</sub>/<i>n</i> with unit‑cell parameters <i>a</i> = 17.8494(15) Å, <i>b</i> = 10.2272(9) Å, <i>c</i> = 18.7853(16) Å, β = 92.9220(10)<sup>°</sup>, <i>V</i> = 3424.8(5) Å<sup>3</sup>, and <i>Z</i> = 4. Refinement converged to <i>R</i> = 0.0525 and ω<i>R</i> = 0.1283 for 5094 observed reflections [<i>I</i> &gt; 2σ(<i>I</i>)].</p>

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Reactions of (p-Cymene)Ru(S2C2B10H10) with 1,1-Diphenyl-2-Propyn-1-Ol: Synthesis and Structural Diversity of Novel Carborane-Incorporating Ruthenium Complexes

  • 期刊论文

  • 发表日期：

    2026年3月11日

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  • J. R. Hu

摘要

Abstract

The reaction of the dinuclear precursor [(p‑cymene)RuCl2]2 with ortho‑carborane, elemental sulfur and 1,1‑diphenyl‑2‑propyn‑1‑ol (HC≡CC(OH)Ph2) yields two carborane‑incorporating ruthenium complexes via divergent pathways. Besides the known B–H activation product (p‑cymene)Ru[H9B10C2S2CH2CC(OH)Ph2] (2), a novel complex (p‑cymene)Ru(H10B9C2S2CHCCPh2) (1) was isolated and fully characterized. Its formation proceeds through initial dehydration of the alkynol to give an allenylidene intermediate, followed by attack of two sulfur atoms at the C=C=CPh2 unit and concomitant extrusion of one boron atom from the closo‑C2B10H10 cage, resulting in a rare nido‑C2B9 metallacyclic framework. Complex 1 was characterized by IR, NMR, MS, elemental analysis, and single‑crystal X‑ray diffraction. It crystallizes in the monoclinic space group P21/n with unit‑cell parameters a = 17.8494(15) Å, b = 10.2272(9) Å, c = 18.7853(16) Å, β = 92.9220(10)°, V = 3424.8(5) Å3, and Z = 4. Refinement converged to R = 0.0525 and ωR = 0.1283 for 5094 observed reflections [I > 2σ(I)].