摘要
Reaction of SmI2(THF)x with 2 equivalents of NaOAr (Ar = C6H2-tert-Bu3-2,4,6) in THF affords a divalent complex of Sm(OAr)2(THF)yTHF 1 in 90.8% yield. Treatment of 1 with 1,2-dimethoxyethane (DME) leads to the ligand-exchange reaction, and a DME-solvated complex of Sm(OAr)2(DME)2 2 was obtained. Complex 1 crystallizes in monoclinic, space group P21/c with a = 10.366(5), b = 33.024(15), c = 16.123(7) A, β = 93.197(8)°, V = 5511 (4) A^3, Z = 4, C52H90O6Sm, Mr = 961.59, Dc = 1.159 g/cm^3, F(000) = 2048,μ(MoKα) = 1.107 mm^-1, R = 0.0844 and wR = 0.1401 for 4694 observed reflections. Complex 2 crystallizes in monoclinic, space group C2/c with a = 27.222(5), b = 10.6140(19), c = 17.398(4) A, β = 110.245(3)°, V = 4716.4(16) A^3, Z = 4, C44H78O6Sm, Mr = 853.41, Dc = 1.202 g/cm^3, F(000) = 1808,μ(MoKα) = 1.285 mm^-1, R = 0.0361 and wR = 0.0830 for 5210 observed reflections.
Reaction of SmI2(THF)x with 2 equivalents of NaOAr (Ar = C6H2-tert-Bu3-2,4,6) in THF affords a divalent complex of Sm(OAr)2(THF)yTHF 1 in 90.8% yield. Treatment of 1 with 1,2-dimethoxyethane (DME) leads to the ligand-exchange reaction, and a DME-solvated complex of Sm(OAr)2(DME)2 2 was obtained. Complex 1 crystallizes in monoclinic, space group P21/c with a = 10.366(5), b = 33.024(15), c = 16.123(7) A, β = 93.197(8)°, V = 5511 (4) A^3, Z = 4, C52H90O6Sm, Mr = 961.59, Dc = 1.159 g/cm^3, F(000) = 2048,μ(MoKα) = 1.107 mm^-1, R = 0.0844 and wR = 0.1401 for 4694 observed reflections. Complex 2 crystallizes in monoclinic, space group C2/c with a = 27.222(5), b = 10.6140(19), c = 17.398(4) A, β = 110.245(3)°, V = 4716.4(16) A^3, Z = 4, C44H78O6Sm, Mr = 853.41, Dc = 1.202 g/cm^3, F(000) = 1808,μ(MoKα) = 1.285 mm^-1, R = 0.0361 and wR = 0.0830 for 5210 observed reflections.
基金
The project was supported by the Qinglan Foundation of Jiangsu Province (HB2001-27) and the Foundation of Educational Commission of Jiangsu Province (04KJD560171)