New SO<sub>2</sub> Iron-Containing Cluster Compounds [PPN]<sub>2</sub>[Fe<sub>3</sub>(CO)<sub>9</sub>(μ<sub>3</sub>,η<sup>2</sup>-SO<sub>2</sub>)], [PPN]<sub>2</sub>[Fe<sub>3</sub>(CO)<sub>8</sub>(μ-SO<sub>2</sub>)μ<sub>3</sub>-S], [PPN]<sub>2</sub>[Fe<sub>3</sub>(CO)<sub>8</sub>(μ-SO<sub>2</sub>)(μ<sub>3</sub>-CCO)], and [PPN]<sub>2</sub>[Fe<sub>2</sub>(CO)<sub>6</sub>(μ-SO<sub>2</sub>)<sub>2</sub>] from Heterometal Precursors
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Sulfur dioxide reacts with [PPN]2[MFe3(CO)14] (M = Cr, Mo, W) (PPN = bistriphenylphosphonium iminium) to produce [PPN]2[Fe3(CO)9(μ3,η2-SO2)] (I) and [PPN]2[Fe3(CO)8(μ-SO2)μ3-S] (II), which were characterized by infrared spectroscopy, 13C NMR, and X-ray crystallography. Further reaction of I with sulfur dioxide results in the formation of II in 48% yield. Reaction of SO2 with [PPN]2[Fe4(CO)13] yields [PPN]2[Fe2(CO)6(μ-SO2)2] (III) which was characterized by infrared spectroscopy, 13C NMR, mass spectrometry, and X-ray crystallography. One equivalent of sulfur dioxide with [PPN]2[MFe3(CO)14C] (M = Cr, W) produces [PPN]2[Fe3(CO)8(μ-SO2)(μ3-CCO)] (IV), which on further reaction with SO2 gives the known cluster [PPN]2[Fe3(CO)7(μ-SO2)2(μ3-CCO)] (V). An excess of sulfur dioxide with [MFe3(CO)nC]x- (M = Cr, W: n =13, x = 2; M = Rh: n = 12, x = 1; M = Mn: n = 13, x = 1) produced V as the only identified product. Crystallographic data for I·0.5CH2Cl2: monoclinic, Cc (no. 9), a = 29.7648(3) Å, b = 14.6496(1) Å, c = 21.7620(3) Å, β = 123.397(1)°, V = 7922.3 Å3; Z = 4. Crystallographic data for III·NCCH3: monoclinic P21 (no. 4), a = 10.0295(5) Å, b = 26.356(1) Å, c = 14.1032(7) Å, β = 94.691°, V = 3715.6(3) Å3; Z = 4.
