The coordination mode of 3-hydroxypicolinic acid in oxorhenium (V) complexes. Crystal and molecular structures of (n-Bu4N) [ReOCl3 (HOC5H3NCO2)] and [ReOCl(HOC5H5NCO2)2]
1998
Abstract The reaction of (n-Bu 4 N)[ReOCl 4 ] with 3-hydroxypicolinic acid (HL 1 ) in benzene and ethanol yields the green (n-Bu 4 N) [ReOCl 3 (L 1 )] ( 1 ) and blue [ReOCl(L 1 ) 2 ] ( 2 ) complexes, respectively. Elemental analysis, infrared. 1 H NMR and conductivity results indicate that the ligand L 1− acts as a monoanionic bidentate N,O -donor chelate in these complexes. Complexes 1 and 2 were also characterized by X-ray crystallography. Crystal data: C 22 H 40 Cl 3 N 2 O 4 Re ( 1 ): monoclinic space group P 2 1 / n , a = 8.111(3), b = 20.842(8), c = 16.722(7)A, β = 98.14(3)°, V = 2794(2)A 3 , Z = 4, D calc = 1.638Mg m −3 ; structure solution and refinement based on 2451 reflections (Mo Kα, λ = 0.710 73A) converged at R = 0.044. C 12 H 8 ClN 2 O 7 Re ( 2 ): monoclinic space group P 2 1 / n , a = 7.923(3), b = 10.681(5) c = 16.539(7)A, β = 97.80(3)°, V = 1387(7)A 3 , Z = 4, D calc = 2.461Mg m −3 ; 1899 reflections, R = 0.069.
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