CYCLOMETALATION OF A PENTAFLUOROBENZALDEHYDE AZINE PHOSPHINE VIA A C-F BOND FISSION BY IRIDIUM(I) - CRYSTAL-STRUCTURE OF [IRCL2(CO)(PPH(2)CH(2)C(BU(T))=N-N=CH(C6F4))]
Sd. Perera et al., CYCLOMETALATION OF A PENTAFLUOROBENZALDEHYDE AZINE PHOSPHINE VIA A C-F BOND FISSION BY IRIDIUM(I) - CRYSTAL-STRUCTURE OF [IRCL2(CO)(PPH(2)CH(2)C(BU(T))=N-N=CH(C6F4))], Inorganica Chimica Acta, 233(1-2), 1995, pp. 103-107
Condensation of Z-PPh(2)CH(2)C(Bu(t))=NNH2 (1) with pentafluorobenzald
ehyde gave the azine phosphine Z,E-PPh(2)CH(2)C(Bu(t))=N-N=CH(C6F5) (2
). When 2 was heated in benzene with [IrCl(CO)(2)(p-toluidine)], it ga
ve the cyclometallated dichlorocarbonyliridium(III) complex [IrCl2(CO)
{PPh(2)CH(2)C(Bu(t))=N-N=CH(C6F4)}] (4), the formation of which involv
ed a C-F bond fission. Proton, P-31{H-1}, C-13{H-1} and F-19 NMR data
are given. Crystals of 4 are monoclinic, space group P2(1)/c with a=10
.6313(11), b=16.0243(14), c=17.968(2) Angstrom, beta=100.258(7)degrees
and Z=4, R1(=)0.0299 for 6085 observed reflections with I>2.0 sigma(I
).