A first anhydrous praseodymium benzoate–benzoic acid adduct, Pr(OBz)3(HOBz)2

Add time:08/17/2019    Source:sciencedirect.com

Solvent-free rare-earth benzoates appear not to be known. As benzoic acid (HOBz) is thermally sufficiently stable (dec 370 °C), the direct oxidation of praseodymium metal with benzoic acid is an excellent route to secure the solvent-free benzoate–benzoic acid adduct Pr(OBz)3(HOBz)2. Light green crystals were obtained from praseodymium metal and benzoic acid in a 1:3 molar ratio in a sealed glass ampoule (200 °C, 8 days, 100 °C, 2.5 days). The coordination polymer Pr(OBz)3(HOBz)2 crystallizes in the orthorhombic space group Pcnn with a = 9.755(1), b = 24.859(1), c = 26.531(1) Å, Z = 8, R1 = 0.0588 for I0 > 2σ(I0). In the crystal structure there are six bidentate-bridging benzoate anions and two unidentate benzoic acid molecules coordinating to Pr3+. The linear chains exhibit a paddle-wheel like structure when viewed down the chain. These are packed in the fashion of a hexagonal densest packing of rods. Pr–O distances range from 2.347(3) to 2.568(3) Å with an average of 2.464 Å.

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