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Structural and electrochemical properties of iridium-carbon bonded metalloporphyrins. Characterization of (OEP)Ir(C/sub 8/H/sub 13/) and (OEP)Ir(C/sub 8/H/sub 13/)(CO)

Journal Article · · J. Am. Chem. Soc.; (United States)
DOI:https://doi.org/10.1021/ja00284a030· OSTI ID:7203863

An electrochemical and structural study of (OEP)Ir(C/sub 8/H/sub 13/), where OEP is the dianion of octaethylporphyrin and C/sub 8/H/sub 13/ is the cis-bicyclo(3.3.0)oct-1-yl group, is reported. (OEP)Ir(C/sub 8/H/sub 13/) was found to crystallize in the P anti 1 space group with a = 12.78 A, b = 13.33 A, c = 14.20 A, ..cap alpha.. = 58.75/sup 0/, ..beta.. = 69.57/sup 0/, ..gamma.. = 67.15 A, and z = 2. The Ir atom is displaced only 0.08 A from the porphyrin plane, and the iridinium-carbon bond distance was found to be 1.89 A. This is the first reported crystal structure of an iridium porphyrin complex as well as the first example where a bicyclic ligand is sigma bonded to a metalloporphyrin. Two-dimensional NMR techniques were also performed and demonstrate that the structure of (OEP)Ir(C/sub 8/H/sub 13/) is basically the same in solution as in the solid state. The five coordinate complex reversibly binds with CO to form (OEP)Ir(C/sub 8/H/sub 13/)(CO), and a formation constant of K/sub eq/ = 340 +/- 200 atm/sup -1/ was measured for this ligand binding reaction. In addition, detailed electrochemistry and spectroelectrochemistry of (OEP)Ir(C/sub 8/H/sub 13/)(CO) are reported in nonaqueous media, and a complete electrochemical mechanism for oxidation and reduction of both species is presented. Of particular interest is the fact that (OEP)Ir(C/sub 8/H/sub 13/) provides the first example of a sigma-bonded metalloporphyrin which can be reversibly oxidized at the sigma-bonded axial ligand without a cleavage of the metal-carbon bond.

Research Organization:
Univ. of Houston, TX
OSTI ID:
7203863
Journal Information:
J. Am. Chem. Soc.; (United States), Journal Name: J. Am. Chem. Soc.; (United States) Vol. 108:24; ISSN JACSA
Country of Publication:
United States
Language:
English