Crystal structure of dicarbonyl (μ2-indole-2-carboxylato κ2 O:O′)tris(triphenylarsine-κAs)dirhodium(I) acetone solvate, C68H56As3NO5Rh2
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Date
2024
Journal Title
Journal ISSN
Volume Title
Publisher
De Gruyter
Abstract
Background: The complex was synthesized starting with the reduction of hydrated RhCl3 in DMF which was refluxed for approxi mately 20 min to give a yellow solution of di-μ-chloro-tetra carbonyldirhodium(I), [RhCl(CO)2]2. 5–7 The addition of an equivalent amount of indol-2-carboxylic acid (indol(H2)) to the aforementioned yellow solution followed by addition of ice water yielded the dicarbonylrhodium(I) complex, [RhI(indol)(CO)2] by precipitation. The anion formed by double deprotonation of the indole-2-carboxylic acid (indol(H2)) ligand displays an unprecedented and unex pected mode of coordination with Rh(I) by forming bridging ligand to two rhodium centers; the ketonic oxygen atom coordinating (κO) to the Rh2 atom, while the N,O atoms bind to a second rhodium atom Rh1 atom in the more familiar bidentate (κN,O) fashion. The dinuclear title complex sim plifies as [Rh(indol)(CO)(AsPh3)Rh(CO)(AsPh3)2].8 [Rh(indol)(- CO)(AsPh3)Rh(CO)(AsPh3)2] was synthesized by dissolving [Rh(indol)(CO)2] (0.0412 g, 0.1291 mmol) in 5 cm3 of acetone. Triphenylarsine (AsPh3) (0.0396 g, 0.1291 mmol) was added to the solution with stirring, resulting in the immediate evolution of CO gas. After a few minutes the reaction was completed as determined by IR spectroscopy. Ice water was added drop-wise to the solution. A yellow precipitate was filtered off and dried.
Description
Keywords
Crystal structure, Dicarbonyl, Acetone solvate, Rhodium centers, Oxygen
Citation
Elmakki, M.A., Alexander, O.T., Venter, J.A. and Roodt, A., 2024. Crystal structure of dicarbonyl (μ2-indole-2-carboxylato κ2 O: O′) tris (triphenylarsine-κAs) dirhodium (I) acetone solvate, C68H56As3NO5Rh2. Zeitschrift für Kristallographie-New Crystal Structures, (0).