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Ru2(OAc)4Cl (200 mg, 0.422 mmol) and H 2esp ligands (259 mg, 0.929 mmol) were refluxed in a mixture of H2O (20 mL) and MeOH (30 mL) for 3 h. Upon the removal of most of MeOH, the precipitate formed was collected by filtration and rinsed with water. The crude product was purified on a short silica gel column with EtOAc/hexanes (3:1) to yield a golden burgundy solid (294 mg, 88.0% based on ruthenium, For the purpose of analysis, the product was recrystallized from CH 2Cl2 and dried under vacuum for 2 days. FAB-MS (m/e, based on 101Ru, 756 [M, Cl, Anal. for Ru2(esp)2Cl·0.5CH2Cl2. Found (calcd, C, 46.60 (46.65, H, 5.37 5.42
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2. Found (calcd): C, 46.60 (46.65); H, 5.37 (5.42).
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42449157888
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X-ray diffraction data for crystal 1 were collected on a Broker SMART1000 CCD diffractometer using Mo Kα at 300 K. Crystal data for Ru2(esp)2Cl·CH2Cl2: C 34H44Cl5O9Ru2, fw, 976.08, orthorhombic, Pnma, a, 16.9347(7) Å, b, 21.662(1) Å, c, 11.2152(5) Å, V, 4114.3(3) Å3, Z, 4, Dcalcd, 1.576 g cm -3. Of 20 916 reflections measured, 3729 were unique (R int, 0.064, Least-squares refinement based on 3729 reflections with I ≥ 2σ(I) and 238 parameters led to convergence with final R1, 0.037 and wR2, 0.082
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int = 0.064). Least-squares refinement based on 3729 reflections with I ≥ 2σ(I) and 238 parameters led to convergence with final R1 = 0.037 and wR2 = 0.082.
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