The ytterbium complex of isonicotinoyl hydrazone was synthesized and the structure was determined by X-ray diffraction analysis. The crystal and molecular structure of the title complex [Yb-2(L)(3)](OH)(3) shows that ...The ytterbium complex of isonicotinoyl hydrazone was synthesized and the structure was determined by X-ray diffraction analysis. The crystal and molecular structure of the title complex [Yb-2(L)(3)](OH)(3) shows that the complex has two identical nine-coordinated ytterbium ions with each surrounded by N3O6 donor set, Two ytterbium ions are bridged by three phenolate oxygen atoms, The geometry around each ytterbium ions can be considered as a three-capped trigonal prism.展开更多
The reaction of anhydrous YbCl3 with 1 equiv, of Li2Me2Si（NPh）2 in THF, after workup, yielded a ytterbium（Ⅲ） chloride [{Me2Si（NPh）2Yb}（μ2-CI）（TMEDA）]2·3PhMe （1） （TMEDA=tetramethylethanediamine）. T...The reaction of anhydrous YbCl3 with 1 equiv, of Li2Me2Si（NPh）2 in THF, after workup, yielded a ytterbium（Ⅲ） chloride [{Me2Si（NPh）2Yb}（μ2-CI）（TMEDA）]2·3PhMe （1） （TMEDA=tetramethylethanediamine）. The same reaction followed by treatment with Na-K alloy afforded a new ytterbium（H） complex supported by a bridged diamide with four coordinated LiC1 molecules, [{Me2Si（NPh）2Yb（THF）2}（μ3-CI）（μ4-CI）{Li（THF）}2]2·2THF （2） in high yield. Both complexes were structurally characterized by X-ray analysis to be dimers. Complex 1 was a chlorine-bridged dimer with ytterbium in a distorted octahedral geometry. In complex 2 two [Me2Si（NPh）2Yb（THF）2]- （μ3-CI）[Li（THF）]2 moieties were connected with each other by two μ4-CI bridges to form a ＂chair-form＂ framework.展开更多
Two ytterbium complexes stabilized by phenoxy（quinolinyl）amide ligand 3,5-But2-2-OC6H2CH2N-8-C9H6N （L） were synthesized and characterized. Reaction of anhydrous YbC13 with 1 equiv, of LLi2 in THF gave the ytterbiu...Two ytterbium complexes stabilized by phenoxy（quinolinyl）amide ligand 3,5-But2-2-OC6H2CH2N-8-C9H6N （L） were synthesized and characterized. Reaction of anhydrous YbC13 with 1 equiv, of LLi2 in THF gave the ytterbium chloride [LYbCI（THF）]2 （1） in 73% yield. A further reaction of complex 1 with equimolar of NaN（SiMe3）2 in THF afforded the unexpected heterobimetallic ＂ate＂-complex L2YbNa（THF）2 （2） via a ligand redistribution reaction. Complex 2 could also be prepared in high isolated yield by the reaction of anhydrous YbC13 with 2 equiv, of LNa2 generated in situ. Both complexes 1 and 2 were characterized by IR spectroscopy, elemental analysis, and sin- gle-crystal X-ray diffraction analysis. It was found that complex 2 was an effective catalyst for the addition reaction of aromatic amines to carbodiimides.展开更多
The complex [(ButC5H’4)2YbCl]2, crystallized in the triclinic system,space group P1, with a=8. 392(3), b=9. 402(3), c=12. 418(5) , a=68. 78(3),P= 77. 43(3), γ=86. 41 (3)°, V= 891. 4(5) , Z=1, Dc= 1. 68 g/cm3, M...The complex [(ButC5H’4)2YbCl]2, crystallized in the triclinic system,space group P1, with a=8. 392(3), b=9. 402(3), c=12. 418(5) , a=68. 78(3),P= 77. 43(3), γ=86. 41 (3)°, V= 891. 4(5) , Z=1, Dc= 1. 68 g/cm3, Mr=901. 79, λ=0. 71069, F(000) = 464, μ= 56. 49 cm-1. T= 298 K. Final R=0.073, Rw= 0.081 for 2214 reflections with I> 3σ(I0). The molecule has a dimerstructure with two asymmetrical chlorine bridges. Two Bu5C5H4 and two chlorineatoms around the central atom Yb form a distorted tetrahedral geometry.展开更多
The treatment of the mixture of n-BuLi with 1 equiv.8-aminoquinoline in THF in situ,which reacted further with 1/3 equiv.of YbCl3 in THF,to give the homoleptic lanthanide amide ate complex Yb（NH-C9H6N）4Li（C4H8O）2...The treatment of the mixture of n-BuLi with 1 equiv.8-aminoquinoline in THF in situ,which reacted further with 1/3 equiv.of YbCl3 in THF,to give the homoleptic lanthanide amide ate complex Yb（NH-C9H6N）4Li（C4H8O）2（1）.The crystal structure was determined by X-ray diffraction and the following crystallographic data were obtained：C44H44N8O2YbLi,Mr = 896.85,monoclinic,space group C2/c,a = 7.8384（16）,b = 22.294（5）,c = 22.668（5）,β = 97.614（5）°,V = 3926.3（14）3,Z = 4,Dc = 1.517 g/cm3,F（000）= 1812,μ（MoKα）= 2.431 mm-1,R = 0.0542 and wR = 0.1523 for 3372 observed reflections with I 2σ（I）.The structure of molecule 1 consists of one ytterbium atom,one lithium atom,four 8-aminoquinoline ligands and two THF molecules.The ytterbium atom is coordinated by eight nitrogen atoms of four 8-aminoquinoline ligands,forming a distorted dodecahedral geometry.展开更多
The title complex [Yb2Cu3 （O2CCH2CI ）12 （H2O）8]·2H2O（Mr=1838. 73） crystallized in monoclinic space group P21/c, with a=10. 424 （6 ）, b= 17.953（4）, c=15. 193（4）A, β=100. 18（1）, V=2798（2） A3, Z=2, ...The title complex [Yb2Cu3 （O2CCH2CI ）12 （H2O）8]·2H2O（Mr=1838. 73） crystallized in monoclinic space group P21/c, with a=10. 424 （6 ）, b= 17.953（4）, c=15. 193（4）A, β=100. 18（1）, V=2798（2） A3, Z=2, Dc=2.18 g/cm3, R=0. 066, Rw=0. 081 for 3653 unique reflections with I＞ 3（I）, u=50. 9cm-1, F （000）=1782, in which the Cu and Yb atoms are bridged uniquely bychloroacetate groups. The Cu atoms display two types of coordination spheres, a fourcoordinate distorted square and a five-coordinate square pyramid, and the coordinationgeometry of each Yb atom is a square antiprism.展开更多
The solubilities of Yb(ClO4)3. 3H2O-18C6-C2H5OH ternary system at 25 were invstigated by a semimicro method for study of phase equilibrium. and the refractive indexes of saturated solutions were determined. The behavi...The solubilities of Yb(ClO4)3. 3H2O-18C6-C2H5OH ternary system at 25 were invstigated by a semimicro method for study of phase equilibrium. and the refractive indexes of saturated solutions were determined. The behavior of water in this system during the equilibrium was examined. The results indicate that there are two kinds of complexes formed in the system, their chemical compositions are: Yb(ClO4)3 18C6. 3H2O. 2C2H5OH (I) and Yb(ClO4)3 18C6 3H2O C2H5OH. Both are incongruently soluble in EtOH. The influences of rare earth ions and salt anions on formation of complexes were discussed. The two solid complexes have been prepared, and their composihons and properties have been investigated by chemical analysis, IR, DTG and DSC. According to the DSC, the enthalpies of some steps during the decomposition have been obtained for complexes and .展开更多
Yb(NTO) 3(H 2O) 4]·6H 2O was synthesized by mixing an aqueous solution of lithium 3 nitro 1,2,4 triazol 5 onate(LiNTO) and the dilute nitric acid solution of ytterbium oxide. The crystal structure has be...Yb(NTO) 3(H 2O) 4]·6H 2O was synthesized by mixing an aqueous solution of lithium 3 nitro 1,2,4 triazol 5 onate(LiNTO) and the dilute nitric acid solution of ytterbium oxide. The crystal structure has been determined by a four circle X ray diffractometer. The crystal is monoclinic, space group C2/c with crystal parameters a= 3 6931(5) nm, b =0 6683(10) nm, c =2 5656(3) nm, β =130 974(5)°, V =4 7811(11) nm 3, Z =8, d c=2 013 g·cm -3 , μ =4 017 mm -1 , F (000)=2850. The final R is 0 0258, the coordination number of Yb 3+ is seven and the geometry of the ytterbium complex is pentagonal bipyramid.展开更多
文摘The ytterbium complex of isonicotinoyl hydrazone was synthesized and the structure was determined by X-ray diffraction analysis. The crystal and molecular structure of the title complex [Yb-2(L)(3)](OH)(3) shows that the complex has two identical nine-coordinated ytterbium ions with each surrounded by N3O6 donor set, Two ytterbium ions are bridged by three phenolate oxygen atoms, The geometry around each ytterbium ions can be considered as a three-capped trigonal prism.
基金Project-supported by the National Natural Science Foundation of China （No. 20472063）.
文摘The reaction of anhydrous YbCl3 with 1 equiv, of Li2Me2Si（NPh）2 in THF, after workup, yielded a ytterbium（Ⅲ） chloride [{Me2Si（NPh）2Yb}（μ2-CI）（TMEDA）]2·3PhMe （1） （TMEDA=tetramethylethanediamine）. The same reaction followed by treatment with Na-K alloy afforded a new ytterbium（H） complex supported by a bridged diamide with four coordinated LiC1 molecules, [{Me2Si（NPh）2Yb（THF）2}（μ3-CI）（μ4-CI）{Li（THF）}2]2·2THF （2） in high yield. Both complexes were structurally characterized by X-ray analysis to be dimers. Complex 1 was a chlorine-bridged dimer with ytterbium in a distorted octahedral geometry. In complex 2 two [Me2Si（NPh）2Yb（THF）2]- （μ3-CI）[Li（THF）]2 moieties were connected with each other by two μ4-CI bridges to form a ＂chair-form＂ framework.
基金Project supported by National Natural Science Foundation of China (21072146, 21132002)the Priority Academic Program Development of Jiangsu Higher Education Institutions and Key Laboratory of Organic Synthesis of Jiangsu,Soochow University(KJS1008)for financial support
文摘Two ytterbium complexes stabilized by phenoxy（quinolinyl）amide ligand 3,5-But2-2-OC6H2CH2N-8-C9H6N （L） were synthesized and characterized. Reaction of anhydrous YbC13 with 1 equiv, of LLi2 in THF gave the ytterbium chloride [LYbCI（THF）]2 （1） in 73% yield. A further reaction of complex 1 with equimolar of NaN（SiMe3）2 in THF afforded the unexpected heterobimetallic ＂ate＂-complex L2YbNa（THF）2 （2） via a ligand redistribution reaction. Complex 2 could also be prepared in high isolated yield by the reaction of anhydrous YbC13 with 2 equiv, of LNa2 generated in situ. Both complexes 1 and 2 were characterized by IR spectroscopy, elemental analysis, and sin- gle-crystal X-ray diffraction analysis. It was found that complex 2 was an effective catalyst for the addition reaction of aromatic amines to carbodiimides.
文摘The complex [(ButC5H’4)2YbCl]2, crystallized in the triclinic system,space group P1, with a=8. 392(3), b=9. 402(3), c=12. 418(5) , a=68. 78(3),P= 77. 43(3), γ=86. 41 (3)°, V= 891. 4(5) , Z=1, Dc= 1. 68 g/cm3, Mr=901. 79, λ=0. 71069, F(000) = 464, μ= 56. 49 cm-1. T= 298 K. Final R=0.073, Rw= 0.081 for 2214 reflections with I> 3σ(I0). The molecule has a dimerstructure with two asymmetrical chlorine bridges. Two Bu5C5H4 and two chlorineatoms around the central atom Yb form a distorted tetrahedral geometry.
基金supported by the Ph.D.Programs Foundation (2009BS01)Youth Innovation Foundation (2010SZDYY12)College Students Innovation Foundation (2010SZDX11) of Suzhou Vocational University
文摘The treatment of the mixture of n-BuLi with 1 equiv.8-aminoquinoline in THF in situ,which reacted further with 1/3 equiv.of YbCl3 in THF,to give the homoleptic lanthanide amide ate complex Yb（NH-C9H6N）4Li（C4H8O）2（1）.The crystal structure was determined by X-ray diffraction and the following crystallographic data were obtained：C44H44N8O2YbLi,Mr = 896.85,monoclinic,space group C2/c,a = 7.8384（16）,b = 22.294（5）,c = 22.668（5）,β = 97.614（5）°,V = 3926.3（14）3,Z = 4,Dc = 1.517 g/cm3,F（000）= 1812,μ（MoKα）= 2.431 mm-1,R = 0.0542 and wR = 0.1523 for 3372 observed reflections with I 2σ（I）.The structure of molecule 1 consists of one ytterbium atom,one lithium atom,four 8-aminoquinoline ligands and two THF molecules.The ytterbium atom is coordinated by eight nitrogen atoms of four 8-aminoquinoline ligands,forming a distorted dodecahedral geometry.
文摘The title complex [Yb2Cu3 （O2CCH2CI ）12 （H2O）8]·2H2O（Mr=1838. 73） crystallized in monoclinic space group P21/c, with a=10. 424 （6 ）, b= 17.953（4）, c=15. 193（4）A, β=100. 18（1）, V=2798（2） A3, Z=2, Dc=2.18 g/cm3, R=0. 066, Rw=0. 081 for 3653 unique reflections with I＞ 3（I）, u=50. 9cm-1, F （000）=1782, in which the Cu and Yb atoms are bridged uniquely bychloroacetate groups. The Cu atoms display two types of coordination spheres, a fourcoordinate distorted square and a five-coordinate square pyramid, and the coordinationgeometry of each Yb atom is a square antiprism.
文摘The solubilities of Yb(ClO4)3. 3H2O-18C6-C2H5OH ternary system at 25 were invstigated by a semimicro method for study of phase equilibrium. and the refractive indexes of saturated solutions were determined. The behavior of water in this system during the equilibrium was examined. The results indicate that there are two kinds of complexes formed in the system, their chemical compositions are: Yb(ClO4)3 18C6. 3H2O. 2C2H5OH (I) and Yb(ClO4)3 18C6 3H2O C2H5OH. Both are incongruently soluble in EtOH. The influences of rare earth ions and salt anions on formation of complexes were discussed. The two solid complexes have been prepared, and their composihons and properties have been investigated by chemical analysis, IR, DTG and DSC. According to the DSC, the enthalpies of some steps during the decomposition have been obtained for complexes and .
文摘Yb(NTO) 3(H 2O) 4]·6H 2O was synthesized by mixing an aqueous solution of lithium 3 nitro 1,2,4 triazol 5 onate(LiNTO) and the dilute nitric acid solution of ytterbium oxide. The crystal structure has been determined by a four circle X ray diffractometer. The crystal is monoclinic, space group C2/c with crystal parameters a= 3 6931(5) nm, b =0 6683(10) nm, c =2 5656(3) nm, β =130 974(5)°, V =4 7811(11) nm 3, Z =8, d c=2 013 g·cm -3 , μ =4 017 mm -1 , F (000)=2850. The final R is 0 0258, the coordination number of Yb 3+ is seven and the geometry of the ytterbium complex is pentagonal bipyramid.
