A new long-lived intermediate has been identified in the reaction of iodofo
rm (1) with isopropylmagnesium chloride at -78 degreesC. The structure of t
he symmetrical iodine ate complex 7. I2CH-I-CHI2-MgCl+, has been assigned t
o the deep red intermediate by NMR spectroscopic techniques, supported by c
alculations of (1)J(C-H), (2)J(C-C), and (3)J(C-H) coupling constants.