Some reactions of the title anion were studied.By these reactions six molybdenum complexes were prepared.On reac- tion with 1,3-dibromopropane the anion yielded the cyclic carbene complex(η-C_5H_4Si_2Me_5)MoBr(CO)_2C...Some reactions of the title anion were studied.By these reactions six molybdenum complexes were prepared.On reac- tion with 1,3-dibromopropane the anion yielded the cyclic carbene complex(η-C_5H_4Si_2Me_5)MoBr(CO)_2CO(CH_2)_2CH_2.The crystal and mole- cular structures of (η-C_5H_4Si_2Me_5)MoBr(CO)_3 and 〔(η-C_5H_4Si_2Me_5)Mo- (CO)_3〕_2 Were determined by X-ray crystallography.展开更多
The mixed tris-cyclopentadienyl tetrahydrofuranato samarium complexes bis-(cyclopentadienyl) methylcyclopentadienyl tetrahadrofuranato samarium (Ⅰ) was synthesized by reaction of (C_5H_5)_2SmCl with methyl cyclopenta...The mixed tris-cyclopentadienyl tetrahydrofuranato samarium complexes bis-(cyclopentadienyl) methylcyclopentadienyl tetrahadrofuranato samarium (Ⅰ) was synthesized by reaction of (C_5H_5)_2SmCl with methyl cyclopentadienyl sodium in THF. [(C_5H_5)_2(C_5H_4CH_3)(C_4H_8O)Sm] (Ⅰ) was characterized by elemental analyses, IR spectra and MS spectra. The structure of [(C_5H_5)_2(C_5H_4CH_3)(C_4H_8O)Sm] (Ⅰ), which has two slightly different independent molecules per asymmetric unit, was elucidated through complete X-ray analysis. The crystals are monoclinic with a=1.2791(3) nm, (b=1.0467(2) nm,) c=2.6108(5) nm, β=98.22(2)°, space group Cc, R=0.0381 for 2103 observed reflection with I3σ(I).展开更多
The formation of ( t BuCp) 2ErOEt was discussed. Its single crystal structure was determined by X ray diffraction. The crystal is monoclinic, P 2(1)/ c space group, a =1.0191(2), b =1.6203(5), c ...The formation of ( t BuCp) 2ErOEt was discussed. Its single crystal structure was determined by X ray diffraction. The crystal is monoclinic, P 2(1)/ c space group, a =1.0191(2), b =1.6203(5), c =1.2118(3) nm, β =102.960(10)°, V =1.9500 (nm 3), Z =2, D c=1.566 mg·m -3 , R =0.0450, R w=0.1363. The complex is monomeric and solvent free in the solid state. The erbium ion is coordinated by two tert butyl cyclopentadienyl rings and one oxygen atom of ethoxy group to form a seven coordinated complex.展开更多
Bis （methylcyclopentadienyl） lanthanide amido complex （MeCp） 2YbNPh2 （THF） reacted with n-hexyl isocyanate （n-nexylNCO） in 1：1 molar ratio to give {（MeC5H4）2Yb[OC（NPh2）N（n-hexyl）] }2（1）. Complex 1 was...Bis （methylcyclopentadienyl） lanthanide amido complex （MeCp） 2YbNPh2 （THF） reacted with n-hexyl isocyanate （n-nexylNCO） in 1：1 molar ratio to give {（MeC5H4）2Yb[OC（NPh2）N（n-hexyl）] }2（1）. Complex 1 was characterized by elemental analyses and X-ray diffraction. The title complex belongs to trigonal system and R-3 space group. Its unit cell parameters are a =2.9533（11） nm, b =2.9533（11） nm, c = 1.5873（6） nm, V= 11.9896（80） nm^3, Z =9, Dc= 1.562 mg·m^-3, μ = 3.536 mm^-1（Mo Kα）, F（000） =5670, R =0.034, Rw =0.064. It is a dimeric structure with two symmetrical bridged oxygen atoms. Nitrogen atom is coordinated to the ytterbium atom to form a tricyclic backbone. The coordination number of ytterbium is 9. The whole molecule shows central symmetry.展开更多
A series of new complexes, CpTiCl[S2P(OR)2]2 (where R) Et, n-Pr, i-Pr, Bui, Ph) and CpTiCl [S2POGO]2 (where G) –CH2CMe2CH2-, -CMe2CMe2-) have been prepared by the drop wise addition of the appropriate O, O’-dialkyl ...A series of new complexes, CpTiCl[S2P(OR)2]2 (where R) Et, n-Pr, i-Pr, Bui, Ph) and CpTiCl [S2POGO]2 (where G) –CH2CMe2CH2-, -CMe2CMe2-) have been prepared by the drop wise addition of the appropriate O, O’-dialkyl or -alkylene dithiophosphoric acid to cyclopentadienyl titanium trichloride in 1:2 molar ratio and refluxed in benzene solution. The new compounds were characterized by molecular weight measurements elemental analyses and spectroscopic studies (1H, 13C, and 31P NMR, and in-frared). We suggest a distorted tetrahedron structure of these new complexes and the dithioligand behaves as bidentate ligand.展开更多
The substituted cyclopentadienyl-magnesium-chloride, obtained by exocyclic addition of 6,6-dialkylfulvene and allyl-magnesium-chloride, reacted with the ketone 3, the product was hydrolyzed and dehydrated to give the ...The substituted cyclopentadienyl-magnesium-chloride, obtained by exocyclic addition of 6,6-dialkylfulvene and allyl-magnesium-chloride, reacted with the ketone 3, the product was hydrolyzed and dehydrated to give the 2-(1 ,1-dialkyl-3-butenyl)-6,6-dialkyl-fulvene 5. The structure of 5 was determined by using the 1H NMR spectra of 5 and the adducts of 5 with tetracyanoethylene.展开更多
In recent years,the organometallic ehemistry of the lanthanide metals in low oxidation states has beenactively investigated.The synthesis of the low一valent lanthanide eomPlexes has the signifieant meanings ontheory a...In recent years,the organometallic ehemistry of the lanthanide metals in low oxidation states has beenactively investigated.The synthesis of the low一valent lanthanide eomPlexes has the signifieant meanings ontheory and praeti展开更多
The title compound [(Bu￣tC_5H_4)_2ErCl]_2 crystallized in the triclinic system, space group P1,with a=8.399(2), b=9.429(2), c=12.464(3),a=68.68(2),β= 77.87(2),γ=86.34(2)°,V=897.0(4),Z=1,D_c=1.65g/cm￣3, Mr= 89...The title compound [(Bu￣tC_5H_4)_2ErCl]_2 crystallized in the triclinic system, space group P1,with a=8.399(2), b=9.429(2), c=12.464(3),a=68.68(2),β= 77.87(2),γ=86.34(2)°,V=897.0(4),Z=1,D_c=1.65g/cm￣3, Mr= 890.28,λ=0.71069,F(000)=470, μ=99. 99 cm-1, T=298 K. Final R= 0.0256, R_w=0. 0294 for 2443 reflections with I>3σ(I_0). The molecule is a dimer in which the two (Bu￣tC_5H_4)_2Er units are connected together by two chlorine atoms. The erbium atom is coordinated by two Bu￣tC_5H_4 groups and two chlorine atoms to form a distorted tetrahedron.展开更多
文摘Some reactions of the title anion were studied.By these reactions six molybdenum complexes were prepared.On reac- tion with 1,3-dibromopropane the anion yielded the cyclic carbene complex(η-C_5H_4Si_2Me_5)MoBr(CO)_2CO(CH_2)_2CH_2.The crystal and mole- cular structures of (η-C_5H_4Si_2Me_5)MoBr(CO)_3 and 〔(η-C_5H_4Si_2Me_5)Mo- (CO)_3〕_2 Were determined by X-ray crystallography.
文摘The mixed tris-cyclopentadienyl tetrahydrofuranato samarium complexes bis-(cyclopentadienyl) methylcyclopentadienyl tetrahadrofuranato samarium (Ⅰ) was synthesized by reaction of (C_5H_5)_2SmCl with methyl cyclopentadienyl sodium in THF. [(C_5H_5)_2(C_5H_4CH_3)(C_4H_8O)Sm] (Ⅰ) was characterized by elemental analyses, IR spectra and MS spectra. The structure of [(C_5H_5)_2(C_5H_4CH_3)(C_4H_8O)Sm] (Ⅰ), which has two slightly different independent molecules per asymmetric unit, was elucidated through complete X-ray analysis. The crystals are monoclinic with a=1.2791(3) nm, (b=1.0467(2) nm,) c=2.6108(5) nm, β=98.22(2)°, space group Cc, R=0.0381 for 2103 observed reflection with I3σ(I).
文摘The formation of ( t BuCp) 2ErOEt was discussed. Its single crystal structure was determined by X ray diffraction. The crystal is monoclinic, P 2(1)/ c space group, a =1.0191(2), b =1.6203(5), c =1.2118(3) nm, β =102.960(10)°, V =1.9500 (nm 3), Z =2, D c=1.566 mg·m -3 , R =0.0450, R w=0.1363. The complex is monomeric and solvent free in the solid state. The erbium ion is coordinated by two tert butyl cyclopentadienyl rings and one oxygen atom of ethoxy group to form a seven coordinated complex.
文摘Bis （methylcyclopentadienyl） lanthanide amido complex （MeCp） 2YbNPh2 （THF） reacted with n-hexyl isocyanate （n-nexylNCO） in 1：1 molar ratio to give {（MeC5H4）2Yb[OC（NPh2）N（n-hexyl）] }2（1）. Complex 1 was characterized by elemental analyses and X-ray diffraction. The title complex belongs to trigonal system and R-3 space group. Its unit cell parameters are a =2.9533（11） nm, b =2.9533（11） nm, c = 1.5873（6） nm, V= 11.9896（80） nm^3, Z =9, Dc= 1.562 mg·m^-3, μ = 3.536 mm^-1（Mo Kα）, F（000） =5670, R =0.034, Rw =0.064. It is a dimeric structure with two symmetrical bridged oxygen atoms. Nitrogen atom is coordinated to the ytterbium atom to form a tricyclic backbone. The coordination number of ytterbium is 9. The whole molecule shows central symmetry.
文摘A series of new complexes, CpTiCl[S2P(OR)2]2 (where R) Et, n-Pr, i-Pr, Bui, Ph) and CpTiCl [S2POGO]2 (where G) –CH2CMe2CH2-, -CMe2CMe2-) have been prepared by the drop wise addition of the appropriate O, O’-dialkyl or -alkylene dithiophosphoric acid to cyclopentadienyl titanium trichloride in 1:2 molar ratio and refluxed in benzene solution. The new compounds were characterized by molecular weight measurements elemental analyses and spectroscopic studies (1H, 13C, and 31P NMR, and in-frared). We suggest a distorted tetrahedron structure of these new complexes and the dithioligand behaves as bidentate ligand.
基金Supported by the National Natural Science Foundation of Shandong Province
文摘The substituted cyclopentadienyl-magnesium-chloride, obtained by exocyclic addition of 6,6-dialkylfulvene and allyl-magnesium-chloride, reacted with the ketone 3, the product was hydrolyzed and dehydrated to give the 2-(1 ,1-dialkyl-3-butenyl)-6,6-dialkyl-fulvene 5. The structure of 5 was determined by using the 1H NMR spectra of 5 and the adducts of 5 with tetracyanoethylene.
文摘In recent years,the organometallic ehemistry of the lanthanide metals in low oxidation states has beenactively investigated.The synthesis of the low一valent lanthanide eomPlexes has the signifieant meanings ontheory and praeti
文摘The title compound [(Bu￣tC_5H_4)_2ErCl]_2 crystallized in the triclinic system, space group P1,with a=8.399(2), b=9.429(2), c=12.464(3),a=68.68(2),β= 77.87(2),γ=86.34(2)°,V=897.0(4),Z=1,D_c=1.65g/cm￣3, Mr= 890.28,λ=0.71069,F(000)=470, μ=99. 99 cm-1, T=298 K. Final R= 0.0256, R_w=0. 0294 for 2443 reflections with I>3σ(I_0). The molecule is a dimer in which the two (Bu￣tC_5H_4)_2Er units are connected together by two chlorine atoms. The erbium atom is coordinated by two Bu￣tC_5H_4 groups and two chlorine atoms to form a distorted tetrahedron.
