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Trivalent group 13 metal complexes of N-substituted-3-hydroxy-2-methyl-4-pyridinones Simpson, Linda

Abstract

The compounds tris(N-ռ-propyl-3-hydroxy-2-methyl-4-pyridinonato) aluminum(III), -gallium(III), and -indium(III) and tris(N-ռ-butyl-3-hydroxy-2-methyl-4-pyridinonato)aluminum(III), -gallium(III), and -indium(III) were synthesized. All six compounds were prepared via the metal template effect. They were characterized by IR, FAB-MS, ¹H NMR, ²⁷Al NMR, and elemental analysis. Three of the six complexes were studied by single-crystal X-ray diffraction. They formed trihydrates, unlike their N-methyl and N-ethyl analogues, which formed dodecahydrates. The ռ-butyl complex Al(C₁₀H₁₄N0₂)₃‧3H₂0 (1) and ռ-propyl complexes Al(C₉H₁₂N0₂)₃‧3H₂0 [2], and Ga(C₉H₁₂N0₂)₃‧3H₂0 {3} were basically isostructural, crystallizing in the space group P3 with the following crystal parameters for 1, [2], and {3}: α= 15.885 (1) ([15.328 (1)], {15.367 (2)}) Å, c = 7.280 (8) ([7.2321 (2)], {7.256 (2)}) Å, Z = 2. The data were refined by using 1280 ([1377], {1802}) reflections with I>3σ(I) to R and Rա values of 0.047 ([0.057], {0.055)) and 0.061 ([0.077], {0.081}), respectively. The complexes exist as the rigidly fac geometries with infinite chains of hydrogen bonds parallel to the c axis.

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