Fluorosulfates of the noble metals, part 4 fluorosulfates of iridium

Superacid Anions: Crystal and Molecular Structures of Oxonium Undecafluorodiantimonate(V), [H3O][Sb2F11], Cesium Fluorosulfate, CsSO3F, Cesium Hydrogen Bis(fluorosulfate), Cs[H(SO3F)2], Cesium Tetrakis(fluorosulfato)aurate(III), Cs[Au(SO3F)4], Cesium Hexakis(fluorosulfato)platinate(IV), Cs2[Pt(SO3F)6], and Cesium Hexakis(fluorosulfato)antimonate(V), Cs[Sb(SO3F)6]

“…In summary the vibrational spectra obtained for Cs[Sb(SO 3 F) 6 ] and Cs 2 [Pt(SO 3 F) 6 ] are consistent with the molecular structures reported here and compare well to vibrational spectra reported for a wide range of salts of the type Cs 2 [M(SO 3 F) 6 ], where M = Sn, Ge, Ti, Zr, Hf, Pd, Ir, and Ru where the anion appears to have an oligomeric structure.…”

Synthesis, Molecular Structure, and Vibrational Spectra of mer-Tris(carbonyl)iridium(III) Fluorosulfate, mer-Ir(CO)3(SO3F)3

“…Iridium(III) fluorosulfate, Ir(SO 3 F) 3 is obtained by oxidation of iridium metal with S 2 O 6 F 2 in HSO 3 F at 120 to 140 °C. The earlier report is substantially modified and details are described below. Carbon monoxide (CP grade 99.5% purity) was obtained from Linde Gases and passed through a glass trap cooled to 77 K, to retain moisture and other impurities.…”

“…(iii)The Synthesis of Ir(CO) 3 (SO 3 F) 3 . Iridium metal was oxidized, initially to Ir(SO 3 F) 4 , by reaction with a large excess of S 2 O 6 F 2 in HSO 3 F at ∼120 °C over several weeks as described previously . To ensure complete oxidation of iridium a two-part reactor, shown in Figure , was employed.…”

“…The dark brown solution in part B was heated to 140 °C for 12 more hours to ensure complete oxidation. At this stage the color of the solution changed to a deep blue-purple due to a decomposition of Ir(SO 3 F) 4 to Ir(SO 3 F) 3 . The solution was then transferred by decanting to reactor arm A for the carbonylation reaction.…”

Coordinated trifluoromethanesulfonate and fluorosulfate

“…Various Ir-(III) and Ir(IV) complexes derive from extended reactions in S206F2/FS03H, namely Ir(S03F)3, Ir(S03F)4, and Ir(S03F)62~. 74 Metal carbonates react according to 2MC03 + S206F2 -2M0(FS03) + 2C02 (18) for M = Mn, Co, and Ni, while Ag20(FS03) forms from Ag2C03 in a like manner. 183 Similarly, cerium(III) carbonate yields CeO(FS03) with covalent FS03-.184…”