Metal complex of buckminsterfullerene, (η2-C60)[Pt(PPh3)2]8,has been synthe-sized for the first time. It has been characterized by IR, XPS spectra as well as elementary analysis. The results show that the number bond...Metal complex of buckminsterfullerene, (η2-C60)[Pt(PPh3)2]8,has been synthe-sized for the first time. It has been characterized by IR, XPS spectra as well as elementary analysis. The results show that the number bonded Pt(PPh3)2 to C60 is 8.展开更多
以乙醇为溶剂、RhCl3.3H2O为铑源、三苯基膦(PPh3)为配体及甲醛为羰基源,在常压回流条件下一步法合成目标铑膦配合物HRh(CO)(PPh3)3,考察了不同氢源(H2、NaBH4和KOH)对铑膦配合物结构的影响.利用FT-IR、31P CP MAS NMR和XPS等对不同氢...以乙醇为溶剂、RhCl3.3H2O为铑源、三苯基膦(PPh3)为配体及甲醛为羰基源,在常压回流条件下一步法合成目标铑膦配合物HRh(CO)(PPh3)3,考察了不同氢源(H2、NaBH4和KOH)对铑膦配合物结构的影响.利用FT-IR、31P CP MAS NMR和XPS等对不同氢源条件下制备的铑膦配合物产物的结构进行表征.结果显示:以H2为氢源时,铑膦配合物产物主要为trans-RhCl(CO)(PPh3)2;以NaBH4为氢源时,产物为trans-RhCl(CO)(PPh3)2和HRh(CO)(PPh3)3的混合产物,同时甲醛溶液的滴加速度对产物的组成也有着重要影响,通过控制甲醛溶液的滴加速度可以有效抑制产物中trans-RhCl(CO)(PPh3)2的含量;以KOH为氢源时,产物为目标产物HRh(CO)(PPh3)3.展开更多
Treatment of complex [（μ-SCH2）2NCH2Ph]Fe2（CO）6 with PPh3 in the presence of decarbonylating agent Me3NO-2H2O afforded the rifle complex [（μ-SCH2）2NCH2Ph]Fe2（CO）5（PPh3） in 70% yield. The new complex was cha...Treatment of complex [（μ-SCH2）2NCH2Ph]Fe2（CO）6 with PPh3 in the presence of decarbonylating agent Me3NO-2H2O afforded the rifle complex [（μ-SCH2）2NCH2Ph]Fe2（CO）5（PPh3） in 70% yield. The new complex was characterized by elemental analysis, IR, and 1H （31p, 13C） NMR spectroscopic techniques as well as by X-ray crystallography. It crystallizes in triclinic, space group P i with a = 9.3016（19）, b = 12.698（3）, c = 13.904（3） A, V = 1519.8（7） A3, Z = 2, C32H26Fe2NOsPS2, Mr = 711.33, Dc = 1.554 g/cm3, μ（MoKa） = 1.187 mm^-1, F（000） = 728, T= 113（2） K, the final R = 0.0288 and wR = 0.0680 for 3982 observed reflections （I 〉 2σ（I））. The PPh3 ligand resides in an axial position of the square-pyramidal geometry of the neighboring Fe atom and trans to the benzene ring in order to minimize the steric repulsion between PPh3 and the benzene ring.展开更多
The title compounds 3-（3,5-bis（trifluoromethyl）phenyl）quinoline （1） and 3-（4- fluoro-3-methylphenyl）quinoline （2） were synthesized through Suzuki-Miyaura Cross coupling reaction of 3-bromoquinoloine with ary...The title compounds 3-（3,5-bis（trifluoromethyl）phenyl）quinoline （1） and 3-（4- fluoro-3-methylphenyl）quinoline （2） were synthesized through Suzuki-Miyaura Cross coupling reaction of 3-bromoquinoloine with aryl boronic acids. The title compounds were characterized by single-crystal X-ray diffraction, 1H NMR, 13C NMR, El-MS, elemental analysis and IR. The crystals of 3-（3,5-bis（trifluoromethyl）phenyl）quinoline （C17H9F6N, Mr = 341.25） belongs to the monoclinic system, space group P21n, a = 12.3072（13）, b = 4.9378（6）, c = 24.493（2） A, V= 1473.1（3） A3, Z = 4, Dc = 1.539 Mg m-3, 2 - 0.71073A, μ = 0.144 mm^-1, F（000） = 688, the final R = 0.0715 and wR = 0.1873 for 1875 obserwed reflections with I 〉 2σ（I） and the crystal of 3-（4-fluoro-3- methylphenyl）quinoline （C16H12FN, Mr= 237.27） belongs to the orthorhombic system, space group Pca21, a = 23.794（2）, b = 3.9094（3）, c = 25.669（2） A, V = 2387.7（4） A3, Z = 8, D, = 1.320 Mg m-3, 2 = 0.71073 A, μ = 0.088 mm-1, F（000） = 992, the final R = 0.0534 and wR = 0.1188 for 2270 observed reflections with I 〉 2σ（I）.展开更多
文摘Metal complex of buckminsterfullerene, (η2-C60)[Pt(PPh3)2]8,has been synthe-sized for the first time. It has been characterized by IR, XPS spectra as well as elementary analysis. The results show that the number bonded Pt(PPh3)2 to C60 is 8.
文摘以乙醇为溶剂、RhCl3.3H2O为铑源、三苯基膦(PPh3)为配体及甲醛为羰基源,在常压回流条件下一步法合成目标铑膦配合物HRh(CO)(PPh3)3,考察了不同氢源(H2、NaBH4和KOH)对铑膦配合物结构的影响.利用FT-IR、31P CP MAS NMR和XPS等对不同氢源条件下制备的铑膦配合物产物的结构进行表征.结果显示:以H2为氢源时,铑膦配合物产物主要为trans-RhCl(CO)(PPh3)2;以NaBH4为氢源时,产物为trans-RhCl(CO)(PPh3)2和HRh(CO)(PPh3)3的混合产物,同时甲醛溶液的滴加速度对产物的组成也有着重要影响,通过控制甲醛溶液的滴加速度可以有效抑制产物中trans-RhCl(CO)(PPh3)2的含量;以KOH为氢源时,产物为目标产物HRh(CO)(PPh3)3.
基金supported by the National Natural Science Foundation of China(21222301,21528303,21603234,21771186,21171170,and 21601193)the National Basic Research Program of China(2013CB934302)+1 种基金the Innovative Program of Development Foundation of Hefei Center for Physical Science and Technology(2014FXCX002)the CAS/SAFEA International Partnership Program for Creative Research Teams~~
基金Supported by the start-up foundation of Ningbo University of Technologythe National Natural Science Foundation of China (20902051,21002090)+1 种基金Foundation of the Education Committee of Zhejiang Province (Z200906833)the Natural Science Foundation of Ningbo city (2010A610186)
文摘Treatment of complex [（μ-SCH2）2NCH2Ph]Fe2（CO）6 with PPh3 in the presence of decarbonylating agent Me3NO-2H2O afforded the rifle complex [（μ-SCH2）2NCH2Ph]Fe2（CO）5（PPh3） in 70% yield. The new complex was characterized by elemental analysis, IR, and 1H （31p, 13C） NMR spectroscopic techniques as well as by X-ray crystallography. It crystallizes in triclinic, space group P i with a = 9.3016（19）, b = 12.698（3）, c = 13.904（3） A, V = 1519.8（7） A3, Z = 2, C32H26Fe2NOsPS2, Mr = 711.33, Dc = 1.554 g/cm3, μ（MoKa） = 1.187 mm^-1, F（000） = 728, T= 113（2） K, the final R = 0.0288 and wR = 0.0680 for 3982 observed reflections （I 〉 2σ（I））. The PPh3 ligand resides in an axial position of the square-pyramidal geometry of the neighboring Fe atom and trans to the benzene ring in order to minimize the steric repulsion between PPh3 and the benzene ring.
文摘The title compounds 3-（3,5-bis（trifluoromethyl）phenyl）quinoline （1） and 3-（4- fluoro-3-methylphenyl）quinoline （2） were synthesized through Suzuki-Miyaura Cross coupling reaction of 3-bromoquinoloine with aryl boronic acids. The title compounds were characterized by single-crystal X-ray diffraction, 1H NMR, 13C NMR, El-MS, elemental analysis and IR. The crystals of 3-（3,5-bis（trifluoromethyl）phenyl）quinoline （C17H9F6N, Mr = 341.25） belongs to the monoclinic system, space group P21n, a = 12.3072（13）, b = 4.9378（6）, c = 24.493（2） A, V= 1473.1（3） A3, Z = 4, Dc = 1.539 Mg m-3, 2 - 0.71073A, μ = 0.144 mm^-1, F（000） = 688, the final R = 0.0715 and wR = 0.1873 for 1875 obserwed reflections with I 〉 2σ（I） and the crystal of 3-（4-fluoro-3- methylphenyl）quinoline （C16H12FN, Mr= 237.27） belongs to the orthorhombic system, space group Pca21, a = 23.794（2）, b = 3.9094（3）, c = 25.669（2） A, V = 2387.7（4） A3, Z = 8, D, = 1.320 Mg m-3, 2 = 0.71073 A, μ = 0.088 mm-1, F（000） = 992, the final R = 0.0534 and wR = 0.1188 for 2270 observed reflections with I 〉 2σ（I）.
