Compartmental ligands. Part 8. Metal complexes of ligands derived from 2,3-dihydro-2-hydroxy-4H-1-benzopyran-4-one and α,ω-diamines: crystal and molecular structures of two mononuclear nickel(II) and one mononuclear copper(II) complexes

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Abstract
Compartmental Schiff-base ligands have been prepared from 2,3-dihydro-2-hydroxy-4H-1-benzopyran-4-one and alkane-α,ω-diamines. Mononuclear copper(II), nickel(II), cobalt(II), and dioxouranium(VI) complexes have been prepared and the site occupancy established: the nickel(II) and cobalt(II) are N2O2, the dioxouranium(VI) is O2O2, and positional isomers are available for copper(II). Homobinuclear copper(II), nickel(II), and oxovanadium(IV) complexes were prepared, as were heterobinuclear complexes containing copper(II) and dioxouranium(VI), and nickel(II) and dioxouranium(VI). Three-dimensional X-ray crystal structure analyses have been carried out on {3,3′-(ethane-1,2-diyl-di-imino)bis[1-(o-hydroxyphenyl)-prop-2-enonato]-(N,N′,O1O1′)}nickel(II), (8a; M = Ni), {3,3′-(propane-1,3-diyldi-imino)bis[1-(o-hydroxyphenyl)prop-2-enonato](N,N′,O1,O1′)}copper(II), (8b; M = Cu), and the related complex {3,3′-(ethane-1,2-diyldi-imino)bis[1-(o-hydroxyphenyl)but-2-enonato](N,N′,O1,O1′)}nickel(II), (10). Two crystallographically independent molecules were found for (10). Complex (8a; M = Ni) has Z= 8 in a monoclinic cell with space group C2/c(no. 15, C6 2h), and dimensions a= 23.373(13), b= 7.800(1), c= 20.819(6)Å, β= 110.14(4)°; R= 0.1341 for 603 reflections. Complex (8b; M = Cu) has Z= 8 in a monoclinic cell with space group C2/c(no. 15, C6 2h) and dimensions a= 23.098(18), b= 9.525(5), c= 18.046(8)Å, β= 104.15(5)°; R= 0.1063 for 891 reflections. Complex (10) has Z= 16 in a monoclinic cell with space group B21/c(a non-standard setting of P21/c, no. 14, C5 2h) and dimensions a= 26.11(4), b= 7.797(4), c= 38.42(6)Å, β= 93.656(8)°; R= 0.0376 for 4 344 reflections.

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