Ortho-metalation and carboxylate coordination in the reaction between the dipotassium salt of phthalic acid and Cp*Ir(PMe3)Cl-2: X-ray diffraction structure of Cp*Ir(PMe3)[C6H3(CO2)(CO2H)]

摘要

The cyclopentadienyl complex Cp*Ir(PMe3)Cl-2 reacts with the dipotassium salt of phthalic acid in the presence of AgPF6 via chloride substitution to give the ortho-metalated compound Cp*Ir(PMe3)[C6H3(CO2)(CO2H)]. This new compound has been isolated by recrystallization and has been characterized in solution by H-1 and C-13 NMR spectroscopies, and the solid-state structure has been verified by X-ray crystallography. Cp*Ir(PMe3)[C6H3(CO2)(CO2H)] crystallizes in the monoclinic space group P2(1)/c, a = 9: 1010(6) Angstrom, b = 16.715(1) Angstrom, c = 14.3965(9) Angstrom, beta = 108.24(1)degrees, V = 2080.0(2) Angstrom(3), Z = 4, and d(calc) = 1.813 mg/m(3); R = 0.0276, R-w = 0.0810 for 2730 reflections with I > 2sigma(I). Coordination of the benzene ring to the iridium center via one of the carboxylate groups and ortho-metalation of the C - H moiety that was alpha to the iridium-bound carboxylate group is confirmed. [References: 35]