Citation: QIU Wei-Ren, ZHOU Hai-Rong, FAN Ling-Ling, WANG Yao-Rong, YAO Ying-Ming, SHEN Qi. Syntheses and Crystal Structures of Homleptic Lanthanide Complexes [C6H5COCHC(CH3)N-(p-ClC6H4)]3Ln(THF)n (Ln=Yb, Y, Nd)[J]. Chinese Journal of Structural Chemistry, ;2014, 33(7): 1031-1036.
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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) Å, α=111.996(9), β=91.570(7), γ=93.744(6)°, V=2159.4(13) Å3, Z=2, Dc=1.515 g/cm3, 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) Å, α=112.362(13), β=91.949(11), γ=93.678(14)°, V=2173(2) Å3, 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) Å, α=66.493(13), β=88.61(2), γ=86.664(19)°, V=2279.4(9) Å3, 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.
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Keywords:
- organolanthanide,
- β-ketoiminate ligand,
- crystal structure
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