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The synthesis and chemistry of organoiridium allyl and oxo complexes

Technical Report ·
OSTI ID:5528123

Cp*Ir(eta/sup 3/-C/sub 3/H/sub 5/)H (2, Cp* = eta/sup 5/-C/sub 5/Me/sub 5/) was cleanly synthesized. Thermolysis of 2 in benzene in the presence of phosphines produced Cp*(PR/sub 3/)Ir(n-C/sub 3/H/sub 7/)(C/sub 6/H/sub 5/) (R = Me, Ph), and in hydrocarbon solvents gave substituted ..pi..-allyliridium hydride species. Two mono- and dinuclear cyclometallated complexes were isolated. Thermolysis of Cp*(eta/sup 3/-C/sub 3/H/sub 5/)IrH in concentrated benzene solutions produced Cp*(C/sub 6/H/sub 5/)Ir(..mu..-H)(eta/sup 1/,eta/sup 3/-C/sub 3/H/sub 4/)IrCp*. The structure was determined crystallographically. Addition of dative ligands to 1 produced benzene and Cp*(L)Ir(eta/sup 1/,eta/sup 3/-C/sub 3/H/sub 4/)IrCp* (2-6, L = PMe/sub 3/, CO, CH/sub 2/=CH/sub 2/, P(OMe/sub 3/)/sub 3/ and t-BuNC). Thermolysis of the PMe/sub 3/ complex 2 gave rise to the intramolecular C-H bond activation product. Addition of LiEt/sub 3/BH to Cp*(PMe/sub 3/)(eta/sup 1/-C/sub 3/H/sub 5/)IrCl produces the iridacyclobutane complex Cp*(PMe/sub 3/)IrCH/sub 2/CH/sub 2/CH/sub 2/. Dehydration of (Cp*Ir(..mu..-OH)/sub 3/IrCp*)/sup +/OAc/sup -/ with amine bases generated the bis-..mu..-oxo complex (Cp*IrO)/sub 2/. Addition of PPh/sub 3/ to 1 produced O=PPh/sub 3/ and Cp*(PPh/sub 3/)Ir(..mu..-O)Cp*Ir. The structure was determined crystallographically. 22 refs., 23 figs., 4 tabs.

Research Organization:
Lawrence Berkeley Lab., CA (USA)
DOE Contract Number:
AC03-76SF00098
OSTI ID:
5528123
Report Number(s):
LBL-24230; ON: DE88004558
Country of Publication:
United States
Language:
English

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