Syntheses and Crystal Structures of Homleptic Lanthanide Complexes C6H5COCHC(CH3)N-(p-ClC6H4)3Ln(THF)n (Ln =Yb, Y, Nd)

摘要

Three homoleptic lanthanide complexes, [C6H5COCHC(CH3)N(p-ClC6H4)]3Ln(THF)n(n = 0, Ln = Yb(1); n = 0, Ln = Y(2); n = 1, Ln = Nd(3)), were synthesized by amine elimination reaction of Ln[N(SiMe3)2]3 with 1-phenyl-3-N-(p-chlorophenylimino)-1-butanone. These complexes crystallize in triclinic, space group P1 with a = 9.805(3), b = 14.831(6), c = 16.075(6) A, α = 111.996(9), β = 91.570(7), γ = 93.744(6)°, V = 2159.4(13) A3, Z = 2, D3 c = 1.515 g/cm, F(000) = 986, μ(MoKα) = 2.396 mm-1, R = 0.0360 and wR = 0.0850 for 9548 observed reflections with I > 2σ(I) for complex 1; a = 9.861(5), b = 14.852(9), c = 16.111(9) A, α = 112.362(13), β = 91.949(11), γ = 93.678(14)°, V = 2173(2) A3, Z = 2, Dc = 1.377 g/cm3, F(000) = 924, μ(MoKα) = 1.570 mm-1, R = 0.0735 and wR = 0.1389 for 8015 observed reflections with I > 2σ(I) for complex 2; and a = 9.308(3), b = 15.357(3), c = 17.419(4) A, α = 66.493(13), β = 88.61(2), γ = 86.664(19)°, V = 2279.4(9) A3, Z = 2, Dc = 1.499 g/cm3, F(000) = 1046, μ(MoKα) = 1.364 mm-1, R = 0.0843 and wR = 0.2280 for 8433 observed reflections with I > 2σ(I) for complex 3. Each central metal in complexes 1 and 2 is six-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands to give a distorted octahedral geometry, while the central metal in 3 is seven-coordinated by three nitrogen and three oxygen atoms from three β-ketoiminate ligands and one oxygen atom from the solvated THF molecule to complete a distorted monocapped trigonal prism.