Reactions of 1,3-diisopropylcarbodiimide with alkali metal amides, MN（SiMe3）2 （M=Li or Na） in hexane or THF produced the alkali metal guanidinates { （i-PrN）2C [N（SiMe3）2]Li }2 （1） and { （i-PrN）2C[N（SiMe3...Reactions of 1,3-diisopropylcarbodiimide with alkali metal amides, MN（SiMe3）2 （M=Li or Na） in hexane or THF produced the alkali metal guanidinates { （i-PrN）2C [N（SiMe3）2]Li }2 （1） and { （i-PrN）2C[N（SiMe3）2]Na（THF） } 2 （2） in nearly quantitative yields. Both complexes 1 and 2 were well characterized by elemental analysis, IR spectra, ^1H and ^13C NMR spectra, and X-ray diffraction. It was found that the guanidinates adopt different coordination modes in these complexes.展开更多
A homoleptic lanthanide guanidinate complex [（CH2）5NC（NiPr）2]3Yb was synthesized by the metathesis reaction of lithium guanidinate with anhydrous YbCl3 in 3∶1 molar ratio in THF.Its crystal structure was determin...A homoleptic lanthanide guanidinate complex [（CH2）5NC（NiPr）2]3Yb was synthesized by the metathesis reaction of lithium guanidinate with anhydrous YbCl3 in 3∶1 molar ratio in THF.Its crystal structure was determined by X-ray diffraction.The crystallographic data:C36H72N9Yb,Mr=804.07,orthorhombic,space group P212121（#19）,a=10.3168（7）,b=11.443（7）,c=35.5649（2）?,V=4199.1（5）?3,Z=4,Dc=1.272 g/cm3,F（000）=1684.00,T=193.1K,λ（MoKα）=0.7107?,μ=22.61 cm-1,R=0.040,wR=0.126 for 8653 observed reflections with（I>3.00 σ（I））.The ytterbium is six-coordinate by six nitrogen atoms of three chelation bidentate guanidinate ligands.展开更多
A new dianionic guanidinate bridged diamide ytterbium(Ⅲ) complex {[Me2Si(NPh)2]2Yb[(NiPr)2CN(SiMe3)2]}{Li(THF)2}2 was synthesized by the reaction of bisguanidinate ytterbium chloride [(SiMe3)2NC(NiPr)2]2Yb(μ-Cl)2Li(...A new dianionic guanidinate bridged diamide ytterbium(Ⅲ) complex {[Me2Si(NPh)2]2Yb[(NiPr)2CN(SiMe3)2]}{Li(THF)2}2 was synthesized by the reaction of bisguanidinate ytterbium chloride [(SiMe3)2NC(NiPr)2]2Yb(μ-Cl)2Li(THF)2 with silylene-bridged diamide lithium PhLiNSiMe2NLiPh.The complex was characterized by elemental analysis and IR.The molecular structure was further determined by X-ray diffraction techniques.The crystals are monoclinic,space group p 21/c,a=14.0001(8),b=17.6808(9),c=24.9565(16),β=95.994(3),V=6143.8(6)3,Dc=1.287 g/cm3,Z=4.展开更多
基金Project supported by the National Natural Science Foundation of China （Nos. 20632040, 20604023）.
文摘Reactions of 1,3-diisopropylcarbodiimide with alkali metal amides, MN（SiMe3）2 （M=Li or Na） in hexane or THF produced the alkali metal guanidinates { （i-PrN）2C [N（SiMe3）2]Li }2 （1） and { （i-PrN）2C[N（SiMe3）2]Na（THF） } 2 （2） in nearly quantitative yields. Both complexes 1 and 2 were well characterized by elemental analysis, IR spectra, ^1H and ^13C NMR spectra, and X-ray diffraction. It was found that the guanidinates adopt different coordination modes in these complexes.
文摘A homoleptic lanthanide guanidinate complex [（CH2）5NC（NiPr）2]3Yb was synthesized by the metathesis reaction of lithium guanidinate with anhydrous YbCl3 in 3∶1 molar ratio in THF.Its crystal structure was determined by X-ray diffraction.The crystallographic data:C36H72N9Yb,Mr=804.07,orthorhombic,space group P212121（#19）,a=10.3168（7）,b=11.443（7）,c=35.5649（2）?,V=4199.1（5）?3,Z=4,Dc=1.272 g/cm3,F（000）=1684.00,T=193.1K,λ（MoKα）=0.7107?,μ=22.61 cm-1,R=0.040,wR=0.126 for 8653 observed reflections with（I>3.00 σ（I））.The ytterbium is six-coordinate by six nitrogen atoms of three chelation bidentate guanidinate ligands.
文摘A new dianionic guanidinate bridged diamide ytterbium(Ⅲ) complex {[Me2Si(NPh)2]2Yb[(NiPr)2CN(SiMe3)2]}{Li(THF)2}2 was synthesized by the reaction of bisguanidinate ytterbium chloride [(SiMe3)2NC(NiPr)2]2Yb(μ-Cl)2Li(THF)2 with silylene-bridged diamide lithium PhLiNSiMe2NLiPh.The complex was characterized by elemental analysis and IR.The molecular structure was further determined by X-ray diffraction techniques.The crystals are monoclinic,space group p 21/c,a=14.0001(8),b=17.6808(9),c=24.9565(16),β=95.994(3),V=6143.8(6)3,Dc=1.287 g/cm3,Z=4.
