Synthesis and Characterization of Novel Iodine(III) Compounds; Crystal Structures of Methoxy(trifluoromethyl)iodine(III) Chloride [CF3I(Cl)OCH3] and Dimethoxy(trifluoromethyl)iodine(III) [CF3I(OCH3)2

Abstract

The reactions of CF3I(Cl)F and CF3IF2 with (CH3)3SiOCH3 lead to the novel iodine(III) compounds CF3I(Cl)OCH3 and CF3I(OCH3)2, respectively. The crystal structure of CF3I(Cl)OCH3 confirms that it is a ternary, trifluoromethyl-substituted iodine(III) derivative. CF3I(Cl)OCH3 crystallizes in the triclinic space group P1¯, with four formula units per unit cell with the dimensions a = 8.164(1), b = 8.802(1), c = 10.237(1) Å and angles α = 97.10(1)°, β = 91.41(1)°, γ = 115.00(1)°. CF3I(OCH3)2 crystallizes in the monoclinic space group P21/n with four formula units per unit cell with a = 6.295(1), b = 15.607(1), c = 7.736(1) Å, and β= 111.44(1)°. Both molecules have been additionally characterized by Raman, IR, and NMR spectroscopy and the experimental results are compared with quantum-mechanically calculated parameters.