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Randles, Michael D.
in Cooperation with on an Cooperation-Score of 37%
Topics
Publications (3/3 displayed)
- 2016Mixed-metal cluster chemistry. 37. Syntheses, structural, spectroscopic, electrochemical, and optical power limiting studies of tetranuclear molybdenum-iridium clusters Dedicated to Professor Jack Lewis, a cluster chemist par excellence.citations
- 2015Syntheses, Electrochemical, Linear Optical, and Cubic Nonlinear Optical Properties of Ruthenium-Alkynyl-Functionalized Oligo(phenylenevinylene) Starscitations
- 2015Phosphine, isocyanide, and alkyne reactivity at pentanuclear molybdenum/tungsten-iridium clusterscitations
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article
Mixed-metal cluster chemistry. 37. Syntheses, structural, spectroscopic, electrochemical, and optical power limiting studies of tetranuclear molybdenum-iridium clusters Dedicated to Professor Jack Lewis, a cluster chemist par excellence.
Abstract
<p>Tetrahedral Mo<sub>2</sub>Ir<sub>2</sub>(μ<sub>3</sub>-CO)(μ-CO)<sub>5</sub>(CO)<sub>4</sub>(η<sup>5</sup>-C<sub>5</sub>H<sub>5</sub>)<sub>2</sub> (1) reacted with P(C<sub>6</sub>H<sub>4</sub>Me-4)<sub>3</sub>, P(C<sub>6</sub>H<sub>2</sub>Me<sub>2</sub>-3,5-OMe-4)<sub>3</sub>, and AsPh<sub>3</sub> to afford the substitution products Mo<sub>2</sub>Ir<sub>2</sub>(μ-CO)<sub>3</sub>(CO)<sub>6</sub>(L)(η<sup>5</sup>-C<sub>5</sub>H<sub>5</sub>)<sub>2</sub> [L = P(C<sub>6</sub>H<sub>4</sub>Me-4)<sub>3</sub> (3), P(C<sub>6</sub>H<sub>2</sub>Me<sub>2</sub>-3,5-OMe-4)<sub>3</sub> (4), AsPh<sub>3</sub> (5)] in fair to good yields, while reaction of 1 with HC≡CSiPr<sup>i</sup><sub>3</sub> proceeded by insertion into the Mo-Mo bond to give the pseudo-octahedral Mo<sub>2</sub>Ir<sub>2</sub>(μ<sub>4</sub>-η<sup>2</sup>-HC<sub>2</sub>SiPr<sup>i</sup><sub>3</sub>)(μ-CO)<sub>4</sub>(CO)<sub>4</sub>(η<sup>5</sup>-C<sub>5</sub>H<sub>5</sub>)<sub>2</sub> (6) in fair yield. While MoIr<sub>3</sub>(μ-CO)<sub>3</sub>(CO)<sub>7</sub>(η<sup>5</sup>-C<sub>5</sub>H<sub>5</sub>) reacted with HC≡CSiMe<sub>3</sub> to give a complex mixture of thus-far-uncharacterized products, its phosphine substitution product MoIr<sub>3</sub>(μ-CO)<sub>3</sub>(CO)<sub>5</sub>(PPh<sub>3</sub>)<sub>2</sub>(η<sup>5</sup>-C<sub>5</sub>H<sub>5</sub>) reacted with the same alkyne via insertion into a Mo-Ir bond to afford the pseudo-octahedral MoIr<sub>3</sub>(μ<sub>4</sub>-η<sup>2</sup>-HC<sub>2</sub>SiMe<sub>3</sub>)(μ-CO)<sub>3</sub>(CO)<sub>4</sub>(PPh<sub>3</sub>)<sub>2</sub>(η<sup>5</sup>-C<sub>5</sub>H<sub>5</sub>) (8) in good yield. Clusters 4, 5 (two isomers), 6 and 8 have been characterized by single-crystal X-ray diffraction studies. Cyclic voltammetric studies of Mo<sub>2</sub>Ir<sub>2</sub>(μ-CO)<sub>3</sub>(CO)<sub>6</sub>(PPh<sub>3</sub>)(η<sup>5</sup>-C<sub>5</sub>H<sub>5</sub>)<sub>2</sub> (2), 3-6 and 8 confirmed the tuning of redox potentials upon phosphines/arsine introduction and alkyne modification. IR spectroelectrochemical studies of 2, 6, and 8 suggest decreasing proclivity for bridging carbonyl ligands following oxidation. Variable temperature <sup>31</sup>P NMR studies of 3 and 4 revealed interconverting isomers in solution, the structures of which are assigned as analogues of the X-ray diffraction-confirmed isomers of 5. Studies of 2-5 using ns pulses and the open-aperture Z-scan technique revealed that all are optical limiters at wavelengths in the visible region.</p>