Section 3: Compound 4 [4] (80 mg, 0.075 mmol) and KC 8 (22 mg, 0.163 mmol) were placed in a reaction tube with a magnetic stirrer. Oxygen-free, dry THF (2 mL) was introduced into the reaction tube by vacuum transfer, and the reaction mixture was stirred at room temperature to produce a yellow solution over 3 h. The solvent was removed in vacuo, and the residue was extracted with degassed hexane. The mixture was filtered to remove the graphite and inorganic salt, and the solution was cooled to À30 8C to produce yellow crystals of 3 (55 mg, 81 %). M.p. 1531541551 H NMR (400.2 MHz,[D 6 ]benzene,TMS): d = 0.40 (s,6 H),0.51 (s,6 H),1.15 (s,18 H),1.17 (s,18 H),1.32 (s,18 H),1.40 ppm (s, 18 H); 13 C{ 1 H} NMR (100.6 MHz, [D 6 ]benzene, TMS): d = À5.1, À4.1, 21.6, 21.9, 22.66, 22.72, 29.7, 30.1, 30.5, 30.7 ppm; 29 Si{ 1 H} NMR (79.5 MHz, [D 6 ]benzene, TMS): d = À23.2 (skeletal Si), 18.2, 26.8, 141.4 (skeletal Si); UV/Vis (hexane): l max (e) = 432 (3300), 326 (4700), 288 (5400), 277 nm (47 000). Elemental analysis (%) calcd for C 36 H 84 Br 2 Si 8 : C 47.96, H, 9.39; found: C 47.71, H 9.22. 2 a: Compound 3 (67 mg, 0.074 mmol) and Na 2 [Fe(CO) 4 ] (80 mg, 0.374 mmol) were placed in a reaction tube with a magnetic stirrer. THF (2 mL) was introduced into the reaction tube by vacuum transfer, and the reaction mixture was stirred at room temperature for 2 days to produce an orange solution. The solvent was removed in vacuo, and the residue was extracted with degassed hexane. The mixture was filtered to remove the salt and residual Na 2 [Fe(CO) 4 ], and the solution was cooled to À30 8C to produce pale yellow crystals of 2 a (28 mg, 42 %). M.p. > 184 8C (decomp); 1 H NMR (400.2 MHz, [D 8 ]THF, TMS): d = 0.32 (s, 12 H), 1.18 ppm (s, 72 H); 13 C{ 1 H} NMR (100.6 MHz, [D 8 ]THF, TMS): d = À3.6, 22.3, 30.5, 221.1 ppm; 29 Si{ 1 H} NMR (79.5 MHz, [D 8 ]THF, TMS): d = À15.8 (skeletal Si), 24.6 ppm; IR (KBr): n ˜CO = 1973, 1922 cm À1 . Elemental analysis (%) calcd for C 39 H 84 FeO 3 Si 8 : C 53.13, H 9.60; found: C 53.56, H 9.61.