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| Naji, M. |
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| Mohamed, Tarek |
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| Ertürk, Emre |
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| Taccardi, Nicola |
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| Petrov, R. H. | Madrid |
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| Rančić, M. |
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| Azevedo, Nuno Monteiro |
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article
Dinuclear and mononuclear chromium acetylide complexes
Abstract
<p>Reaction of trans-Cl <sub>2</sub>Cr(dmpe) <sub>2</sub> (1) [dmpe = 1,2-bis(dimethylphosphanyl)ethane] with 0.5 equiv. of Me <sub>3</sub>Sn-C=C-C=C- SnMe <sub>3</sub> or Me <sub>3</sub>Sn-C=C-C <sub>6</sub>H <sub>4</sub>-C=C- SnMe <sub>3</sub> afforded the dinuclear complexes trans-[Cl(dmpe) <sub>2</sub>Cr=C-C=C-C=Cr(dmpe) <sub>2</sub>Cl] (2), trans-[Cl(dmpe) <sub>2</sub>Cr-C=C-C=C-Cr(dmpe) <sub>2</sub>Cl][SnMe <sub>3</sub>Cl <sub>2</sub>] <sub>2</sub> (2[SnMe <sub>3</sub>Cl <sub>2</sub>] <sub>2</sub>), and trans-[Cl(dmpe) <sub>2</sub>Cr-C=C-C <sub>6</sub>H <sub>4</sub>-C=C-Cr(dmpe) <sub>2</sub>Cl][SnMe <sub>3</sub>Cl <sub>2</sub>] <sub>2</sub> (3[SnMe <sub>3</sub>Cl <sub>2</sub>] <sub>2</sub>), which could be transformed to the 2[PF <sub>6</sub>] <sub>2</sub> and 3[BPh <sub>4</sub>] <sub>2</sub> salts. Substitutions of the chloride groups in 2 were carried out to achieve the corresponding iodo (4) and (trimethylsilyl)alkynyl (5) complexes. Utilizing similar reactions and treatment with only 1 equiv. of the corresponding alkynyl ligand [Me <sub>3</sub>Sn-C=C-R (R = -SnMe <sub>3</sub>, -C <sub>6</sub>H <sub>5</sub>), Me <sub>3</sub>Sn-C=C-C=C-R (R = -SiMe <sub>3</sub>, -SnMe <sub>3</sub>), and Me <sub>3</sub>Sn-C=C-C <sub>6</sub>H <sub>4</sub>-C=C-SnMe <sub>3</sub>] allowed us to prepare a series of mononuclear monoacetylide complexes: trans-[Cl(dmpe) <sub>2</sub>Cr-C=C-R] [R = -SnMe <sub>3</sub>(6),- C <sub>6</sub>H <sub>5</sub>(7)], trans-[Cl(dmpe) <sub>2</sub>Cr-C=C-C=C-R] [R = -SiMe <sub>3</sub>(8),-SnMe <sub>3</sub>(9)], and trans-[Cl(dmpe) <sub>2</sub>Cr-C=C-C <sub>6</sub>H <sub>4</sub>-C=C-SnMe <sub>3</sub>] (10), respectively. The complexes 2, 2[SnMe <sub>3</sub>Cl <sub>2</sub>] <sub>2</sub>, 2[PF <sub>6</sub>] <sub>2</sub>, 3[SnMe <sub>3</sub>Cl <sub>2</sub>] <sub>2</sub>, 3[BPh <sub>4</sub>] <sub>2</sub>, and 6-10 displayed paramagnetic behavior. Electrochemical studies performed on the dinuclear complexes (2), (2[SnMe <sub>3</sub>Cl <sub>2</sub>] <sub>2</sub>), (3[SnMe <sub>3</sub>Cl <sub>2</sub>] <sub>2</sub>), and (5) showed one two-electron redox wave revealing a class-I type behavior based on the Robin-Day classification, which is untypical for dinuclear complexes bridged by a butadiyne ligand. The complexes were characterized by NMR, ESI-MS, cyclic voltammetry, EPR spectroscopy, magnetic measurements, and exemplary single-crystal X-ray diffraction studies for 2, 2[SnMe <sub>3</sub>Cl <sub>2</sub>] <sub>2</sub>, 8, 9, and 10. Chromium dinuclear complexes bridged by C <sub>4</sub> units were obtained in good yields. Physical studies done on the dinuclear complexes revealed a class-I behavior(Robin-Day classification). Related mononuclear chromium monoacetylide complexes were also accessible.</p>