The reaction of anhydrous YbCl3 with lithium b-diketiminate, LLi (L = N,N- diphenyl-2,4-pentanediimine anion), in 1:1 molar ratio in THF gave rise to the title complex LYbCl2(THF)2 1 which has been characterized by si...The reaction of anhydrous YbCl3 with lithium b-diketiminate, LLi (L = N,N- diphenyl-2,4-pentanediimine anion), in 1:1 molar ratio in THF gave rise to the title complex LYbCl2(THF)2 1 which has been characterized by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pna21(#33) with a = 19.657(8), b = 9.581(4), c = 14.107(6) ? V = 2656.8(18) 3, Z = 4, C25H33N2O2Cl2Yb, Mr = 637.49, Dc = 1.594 g/cm3, F(000) = 1268.00 and m(MoKa) = 3.744mm-1. The final R and wR are 0.031 and 0.073 for 2596 observed reflections with I > 2s(I), respectively. The X-ray crystal structure analysis revealed that the center ytterbium(III) is bonded to two chloride anions, two oxygen atoms from two tetrahydrofuran molecules and one chelate ligand b-diketiminate to form a six-coordinate distorted octahedral geometry.展开更多
Reaction of anhydrous YbCl3 with 1 equiv. of LLi [L=p-ClPhNC(Me)CH(Me)N(C6H3-2,6-i-Pr2)] in THF at room temperature gave the b-diketiminate lanthanide dichloride LYbCl2(THF)2 (1) in good isolated yield. Similarly reac...Reaction of anhydrous YbCl3 with 1 equiv. of LLi [L=p-ClPhNC(Me)CH(Me)N(C6H3-2,6-i-Pr2)] in THF at room temperature gave the b-diketiminate lanthanide dichloride LYbCl2(THF)2 (1) in good isolated yield. Similarly reaction of anhydrous YbCl3 with 1 equiv. of LLi, then with 1 equiv. of t-BuCpNa in THF yielded the expected mixed-ligand b-diketiminate ytterbium chloride (t-BuCp)YbL(m-Cl)2Li(THF)2 (2). Both 1 and 2 were well charac-terized by elemental analysis, IR spectra, 1H NMR spectra, and X-ray diffraction analysis.展开更多
基金Supported by the National Natural Science Foundation of China (20072027) Department of Education of Jiangsu province and the Key Laboratory of Organic Synthesis of Jiangsu province
文摘The reaction of anhydrous YbCl3 with lithium b-diketiminate, LLi (L = N,N- diphenyl-2,4-pentanediimine anion), in 1:1 molar ratio in THF gave rise to the title complex LYbCl2(THF)2 1 which has been characterized by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pna21(#33) with a = 19.657(8), b = 9.581(4), c = 14.107(6) ? V = 2656.8(18) 3, Z = 4, C25H33N2O2Cl2Yb, Mr = 637.49, Dc = 1.594 g/cm3, F(000) = 1268.00 and m(MoKa) = 3.744mm-1. The final R and wR are 0.031 and 0.073 for 2596 observed reflections with I > 2s(I), respectively. The X-ray crystal structure analysis revealed that the center ytterbium(III) is bonded to two chloride anions, two oxygen atoms from two tetrahydrofuran molecules and one chelate ligand b-diketiminate to form a six-coordinate distorted octahedral geometry.
基金Project supported by the National Natural Science Foundation of China (No. 20272040) and Ningbo Science and Technology Bureau.
文摘Reaction of anhydrous YbCl3 with 1 equiv. of LLi [L=p-ClPhNC(Me)CH(Me)N(C6H3-2,6-i-Pr2)] in THF at room temperature gave the b-diketiminate lanthanide dichloride LYbCl2(THF)2 (1) in good isolated yield. Similarly reaction of anhydrous YbCl3 with 1 equiv. of LLi, then with 1 equiv. of t-BuCpNa in THF yielded the expected mixed-ligand b-diketiminate ytterbium chloride (t-BuCp)YbL(m-Cl)2Li(THF)2 (2). Both 1 and 2 were well charac-terized by elemental analysis, IR spectra, 1H NMR spectra, and X-ray diffraction analysis.
