Abstract
Methods of metallo-silanol synthesis have been developed. The Ir(I) complex (Et3P)2Ir(C2H4)Cl (1) oxidatively adds secondary silanols R2SiHOH (R = iPr, tBu) to yield the iridium−silanol complexes [(Et3P)2Ir(H)(Cl)(SiR2OH)] (R = iPr, 2; R = tBu, 3). The crystal structure of 2 exhibits a trigonal-bipyramidal geometry, and intermolecular Si−O−H- - -Cl hydrogen bonding is present. Deprotonation of 2 results in the highly thermodynamically stable metallo-silanolate [(Et3P)2Ir(H)(Cl)(SiiPr2OLi)]2 (4). Compound 4 has an almost planar core, consisting of two atoms each of iridium, silicon, chlorine, oxygen, and lithium. Upon treatment of (Et3P)3RhCl with HSiiPr2OH, the first Rh−silanol complex, trans-[(Et3P)2Rh(H)(Cl)(iPrSi2OH)], is formed in an equilibrium with the starting complex (Keq = 4 × 10-3); hence, the reaction is dependent on the concentration of the silanol and Et3P, an excess of the latter shifting the equilibrium to the starting compounds. Reaction of the bis-phosphine complex [(Et3P)2RhCl]2 with the...
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