Routine solution reaction of Gd3＋ and p-phenylenediamine-N,N,N′,N′-tetraacetic acid （p-PhDTA） yields a dinuclear complex [Gd2（ox）（p-PhDTA）2（H2O）10]·6H2O （ox = oxalate）, which was characterized by sin...Routine solution reaction of Gd3＋ and p-phenylenediamine-N,N,N′,N′-tetraacetic acid （p-PhDTA） yields a dinuclear complex [Gd2（ox）（p-PhDTA）2（H2O）10]·6H2O （ox = oxalate）, which was characterized by single-crystal X-ray diffraction （MoKα radiation, = 0.71073）, elemental analysis and IR. This complex crystallizes in the monoclinic system, space group P21/n with a = 10.2522（8）, b = 10.0053（8）, c = 23.8834（18）, = 99.1080（10）°, V = 2419.0（3）3, Z = 2, Mr = 1367.32, Dc = 1.877 g/cm3, F（000） = 1368, = 2.830 mm-1, the final R = 0.0337 and wR = 0.0794 for 4747 observed reflections （I 〉 2 （I））. The exo-tetradentate oxalate ligand, generated in situ from the oxidative coupling of methanol, is incorporated to construct a dinuclear Gd2（ox）2 unit decorated with p-PhDTA ligands on the two sides with a monodentate coordination mode. The dinuclear molecules are further connected by the lattice water molecules to form a three-dimen- sional hydrogen network.展开更多
A 1-D zigzag chain [Sn（edt）2（p-phenylenediamine）], （edt=ethane-l,2-thiolate） was synthesized by self-assembly and determined by X-ray structure analysis. The title compound （C10H16N2S4Sn） crystallizes in monoc...A 1-D zigzag chain [Sn（edt）2（p-phenylenediamine）], （edt=ethane-l,2-thiolate） was synthesized by self-assembly and determined by X-ray structure analysis. The title compound （C10H16N2S4Sn） crystallizes in monoclinic, space group C2/c with a=16.659（2）, b=7.0977（10）, c=12.4421（17） A°,β=96.577（2）°, V= 1461.5（4）A°^3, Z=4, Mr=411.18, Dc=1.869 g/cm^3, F（000）=816,μ=2.300 mm^-1, the final R=0.0332 and wR=0.0837 for 1142 observed reflections （I〉2σ（I））. In the complex, Sn^4＋ ion is six-coordinated with four sulfur atoms of two edt ligands from equatorial positions and two nitrogen atoms of p-phenylenediamine ligands from axial positions. The zigzag chain thus formed is parallel to the a axis.展开更多
基金the National Natural Science Foundation of China (No. 21001030 and 21101032)the Foundation for the Authors of Excellent Doctoral Dissertation of Guangdong Province (No. sybzzxm201048)the "211" Creative Project of Guangdong Province
文摘Routine solution reaction of Gd3＋ and p-phenylenediamine-N,N,N′,N′-tetraacetic acid （p-PhDTA） yields a dinuclear complex [Gd2（ox）（p-PhDTA）2（H2O）10]·6H2O （ox = oxalate）, which was characterized by single-crystal X-ray diffraction （MoKα radiation, = 0.71073）, elemental analysis and IR. This complex crystallizes in the monoclinic system, space group P21/n with a = 10.2522（8）, b = 10.0053（8）, c = 23.8834（18）, = 99.1080（10）°, V = 2419.0（3）3, Z = 2, Mr = 1367.32, Dc = 1.877 g/cm3, F（000） = 1368, = 2.830 mm-1, the final R = 0.0337 and wR = 0.0794 for 4747 observed reflections （I 〉 2 （I））. The exo-tetradentate oxalate ligand, generated in situ from the oxidative coupling of methanol, is incorporated to construct a dinuclear Gd2（ox）2 unit decorated with p-PhDTA ligands on the two sides with a monodentate coordination mode. The dinuclear molecules are further connected by the lattice water molecules to form a three-dimen- sional hydrogen network.
基金This research was supported by the State Key Laboratory of Structural Chemistry, the National Natural Science Foundation of China (20273073, 20333070, 90206040) and Natural Science Foundation of Fujian Province (2004J041, 2003J042, 2004HZ01-1)
文摘A 1-D zigzag chain [Sn（edt）2（p-phenylenediamine）], （edt=ethane-l,2-thiolate） was synthesized by self-assembly and determined by X-ray structure analysis. The title compound （C10H16N2S4Sn） crystallizes in monoclinic, space group C2/c with a=16.659（2）, b=7.0977（10）, c=12.4421（17） A°,β=96.577（2）°, V= 1461.5（4）A°^3, Z=4, Mr=411.18, Dc=1.869 g/cm^3, F（000）=816,μ=2.300 mm^-1, the final R=0.0332 and wR=0.0837 for 1142 observed reflections （I〉2σ（I））. In the complex, Sn^4＋ ion is six-coordinated with four sulfur atoms of two edt ligands from equatorial positions and two nitrogen atoms of p-phenylenediamine ligands from axial positions. The zigzag chain thus formed is parallel to the a axis.
