The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA wi...The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2]（ClO4）E·H2O 1 and [CoL2]（NO3）E·H2O 2 as isolatable products （L= N-（1- benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine）, where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA. Both complexes were characterized by X-ray crystallography. Crystal data for complex 1： monoclinic, space group P21/c, a = 11.9214（10）, b = 23.5828（17）, c = 14.0387（12）A, β = 135.219（4）°, C22H30Cl2CoN8O9, Mr = 680.37, V = 2780.1（4） A^3 ,Z = 4, Dc = 1.625 g/cm^3,μ（MoKa） = 0.876 mm^-1, F（000） = 1404, the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections （I 〉 2σ（I））. Crystal data for complex 2： monoclinic, space group P21/c, a = 18.2162（16）, b = 10.0610（6）, c = 18.593（2）A, β = 130.099（3）°, C22H30CoN10O7, Mr = 605.49, V = 2606.5（4） A3 Z = 4, Dc = 1.543 g/cm^3,μ（MoKa） = 0.722 mm^-1, F（000） = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate iigands L, exhibiting a slightly distorted octahedral coordination sphere. In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4^- （or NO3^-） groups to form a 3D framework. In complex 2, the strong π-π interactions increase the stability of the structure.展开更多
研究了1-磺酰基三氮唑在二聚醋酸铑催化下和2H-氮丙啶发生反应生成一系列苯基取代N-磺酰基-1,2-二氢吡嗪化合物的合成方法。考察了催化剂和溶剂对产物产率的影响。化合物结构经1 H NMR和13 C NMR鉴定和表征。该反应为二氢吡嗪化合物的...研究了1-磺酰基三氮唑在二聚醋酸铑催化下和2H-氮丙啶发生反应生成一系列苯基取代N-磺酰基-1,2-二氢吡嗪化合物的合成方法。考察了催化剂和溶剂对产物产率的影响。化合物结构经1 H NMR和13 C NMR鉴定和表征。该反应为二氢吡嗪化合物的合成提供了一种新颖的途径。展开更多
A new ionic pair complex,1,2′-dinithile-1,2′-dithiolene nickel(II) containing substituted benzylpyridinium [Bz(Me)Py]2[Ni(mnt)2],is prepared and characterized by elemental analyses,IR,UV-VIS and single crystal X-ray...A new ionic pair complex,1,2′-dinithile-1,2′-dithiolene nickel(II) containing substituted benzylpyridinium [Bz(Me)Py]2[Ni(mnt)2],is prepared and characterized by elemental analyses,IR,UV-VIS and single crystal X-ray diffraction.Where [Bz(Me)Py]+ was 1-(1′-phenylethyl)-pyridinium and mnt2-is 1,2′-dinithile-1,2′-dithiolene.The crystal structure was solved by direct method and refined by full-matrix least-squares methods for All the nonhydrogen atoms.The final R1 and wR2 for all data were 0.0450 and 0.1236,respectively.The complex is composed of two [Bz(Me)Py]+ cations and a [Ni(mnt)2]2-anion.The [Ni(mnt)2]2-anions form a stepwise structure by π-π stacking interactions between the CN groups.The cation-anion C-H···N hydrogen bonds and cation-cation C-H···π interactions give further rise to a network structure.展开更多
基金the National Natural Science Foundation of China (20425313)the Natural Science Foundation of Fujian Province (2005HZ01-1, 2006L2005, 2006F3135, 2006J0183)
文摘The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2]（ClO4）E·H2O 1 and [CoL2]（NO3）E·H2O 2 as isolatable products （L= N-（1- benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine）, where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA. Both complexes were characterized by X-ray crystallography. Crystal data for complex 1： monoclinic, space group P21/c, a = 11.9214（10）, b = 23.5828（17）, c = 14.0387（12）A, β = 135.219（4）°, C22H30Cl2CoN8O9, Mr = 680.37, V = 2780.1（4） A^3 ,Z = 4, Dc = 1.625 g/cm^3,μ（MoKa） = 0.876 mm^-1, F（000） = 1404, the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections （I 〉 2σ（I））. Crystal data for complex 2： monoclinic, space group P21/c, a = 18.2162（16）, b = 10.0610（6）, c = 18.593（2）A, β = 130.099（3）°, C22H30CoN10O7, Mr = 605.49, V = 2606.5（4） A3 Z = 4, Dc = 1.543 g/cm^3,μ（MoKa） = 0.722 mm^-1, F（000） = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate iigands L, exhibiting a slightly distorted octahedral coordination sphere. In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4^- （or NO3^-） groups to form a 3D framework. In complex 2, the strong π-π interactions increase the stability of the structure.
基金supported by the Chinese Ministry of Education via the Program for New Century Excellent Talents in University (NCET-12-0079)the Fundamental Research Funds for the Central Universities (DUT12LK51)~~
文摘A new ionic pair complex,1,2′-dinithile-1,2′-dithiolene nickel(II) containing substituted benzylpyridinium [Bz(Me)Py]2[Ni(mnt)2],is prepared and characterized by elemental analyses,IR,UV-VIS and single crystal X-ray diffraction.Where [Bz(Me)Py]+ was 1-(1′-phenylethyl)-pyridinium and mnt2-is 1,2′-dinithile-1,2′-dithiolene.The crystal structure was solved by direct method and refined by full-matrix least-squares methods for All the nonhydrogen atoms.The final R1 and wR2 for all data were 0.0450 and 0.1236,respectively.The complex is composed of two [Bz(Me)Py]+ cations and a [Ni(mnt)2]2-anion.The [Ni(mnt)2]2-anions form a stepwise structure by π-π stacking interactions between the CN groups.The cation-anion C-H···N hydrogen bonds and cation-cation C-H···π interactions give further rise to a network structure.
