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Example 3Preparation of [Mn(hpimp)]2 (A)A solution of the hpimp ligand synthesized according to Example 1 (2.0 g, 9.4 mmol, 1.0 eq) in 150 ml degassed methanol was slowly added drop by drop to a solution of Mn(OAc)2×4H2O (2.3 g, 9.4 mmol, 1.0 eq) in 50 ml degassed methanol. The mixture was then stirred at room temperature for 15 minutes and subsequently heated under reflux for two hours. The mixture was then cooled down to room temperature, the resulting precipitate was centrifuged off, washed three times with degassed methanol and dried under vacuum. Repeated freezing of the flask in liquid nitrogen and subsequent thawing to room temperature under vacuum (freeze drying) afforded the partially agglomerated material as a fine powder.Yield: orange powder, 78%.MALDI-MS: m/z: 266.2 [M]+, 532.2 [(M)2]+.IR-spectroscopy /cm-1: 3414 (w), 3060 (w), 3011 (w), 1607 (s), 1583 (m), 1543 (m), 1472 (s), 1441 (m), 1391 (m), 1298 (s), 1261 (m), 918 (m), 756 (m), 745 (s).Elementary analysis: C13H9MnNO2 (M=266.2)/wt % calculated C: 58.66 H: 3.41 N: 5.26 Mn: 20.6 found C: 57.62 H: 3.83 N: 5.16 Mn: 19.9
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