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Synthesis of Ru2(D(3,5-Cl2Ph)F) 3(D(4-MeOPh-Ph)F)Cl (1c, R·u2(D(3,5- Cl2Ph)F)3(D(I-Ph)F)Cl (0.13 mmol, 4-bromozincanisole (1.0 mmol, and Pd(DPEphos)Cl2 (0.014 mmol) were stirred in 10 mL of THF at room temperature for 1 h under a nitrogen atmosphere. The reaction mixture was filtered through a 2 cm silicon gel pad and subsequently purified on a silica column with hexanes-THF (10:2 v/v) to yield 180 mg of a black crystalline solid (85% based on Ru, Data for 1c are as follows. Anal. Found (caled) for C66H44Cl13N8O 2Ru2·2C4H8O: C, 49.72 (49.70, H, 3.32 (3.38, N, 6.54 6.27
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8O: C, 49.72 (49.70); H, 3.32 (3.38); N, 6.54 (6.27).
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0001097234
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Lin, C.1
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38049118774
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Synthesis of trans-(PhC≡C)2[Ru2(D(3,5- Cl2Ph)F)3(DMBA-Ph, 2a, trans-(PhC≡C) 2[Ru2(D(3,5-Cl2Ph)F)3(DMBA-I, 100 mg, 0.06 mmol) was stirred with BrZnC6H5 (0.5 mmol) and Pd(DPEphos)Cl2 (5 mg, 0.007 mmol) in 5 mL of THF for 2 h at room temperature. The reaction mixture was filtered through a 2 cm silicon gel pad, and the filtrate was purified on a silica column with hexanes-THF (20:1 v/v) to yield 2a as a black crystalline solid (50 mg, 45% based on Ru, Data for 2a are as follows. Anal. Found (calcd) for C70H46Cl 12N8Ru2.3H20: C, 49.99 (50.02, H, 3.26 (3.12, N, 6.58 (6.67, 1H NMR (CDCl3) δ 8.17 (s, 1H, NCHN, 8.00 (s, 2H, NCHN, 7.90 (s, 2H, aromatic, 7.72-7.33 (m, 5H, aromatic, 7.17-6.93 (m, 22H, aromatic, 6.70-6.61 m, 8H, aromatic, 3.68
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3) δ 8.17 (s, 1H, -NCHN), 8.00 (s, 2H, -NCHN), 7.90 (s, 2H, aromatic), 7.72-7.33 (m, 5H, aromatic), 7.17-6.93 (m, 22H, aromatic), 6.70-6.61 (m, 8H, aromatic), 3.68 (s, 6H, Me-NCN-Me).
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