| 两个含N-皮考林酰肼铁配合物的合成和结构表征 |
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| 引用本文： | 吴文士,刘世雄. 两个含N-皮考林酰肼铁配合物的合成和结构表征[J]. 高等学校化学学报, 2003, 24(12): 2137-2142 |
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| 作者姓名： | 吴文士 刘世雄 |
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| 作者单位： | 1. 福州大学中心实验室, 福州 350002;2. 华侨大学材料学院, 泉州 362011 |
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| 基金项目： | 福建省自然科学基金 (批准号 :E0 110 0 10 ,E0 2 10 0 2 6)资助 |
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| 摘 要： | 合成了含N-乙酰皮考林酰肼(简写为Haphz)的铁配合物[Fe2(aphz)2(μ-CH3O)2Cl2]·CH3OH(1,C19H26Cl2Fe2N6O7,Mr=633.06)和含N-苯甲酰皮考林酰肼(简写为Hphphz)的铁配合物Fe(phphz)Cl2(2,C13H10Cl2FeN3O2,Mr=366.99).2个配合物均属三斜晶系,空间群为P
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| 关 键 词： | 晶体结构 皮考林酰肼 铁配合物 |
| 文章编号： | 0251-0790(2003)12-2137-06 |
| 收稿时间： | 2003-04-14 |
Syntheses and Characterization of Two Iron Complexes with N-Picoloylhydrazide |
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| WU Wen-Shi ,,LIU Shi-Xiong. Syntheses and Characterization of Two Iron Complexes with N-Picoloylhydrazide[J]. Chemical Research In Chinese Universities, 2003, 24(12): 2137-2142 |
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| Authors: | WU Wen-Shi LIU Shi-Xiong |
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| Affiliation: | 1. Central Laboratory, Fuzhou University, Fuzhou 350002, China;2. College of Material, Huaqiao University, Quanzhou 362011, China |
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| Abstract: | Two iron complexes with N-acetylpicoloylhydrazide (Haphz) and N-phenylpicoloylhydrazide(Hphphz), [Fe2(aphz)2(μ-CH3OH)2Cl2]·CH3OH(1, C19H26Cl2Fe2N6O7, Mr= 633.06) and Fe(phphz)Cl2(2, C13H10Cl2FeN3O2, Mr=366.99), were synthesized. Complex 1 belongs to a triclinic system, space group P1, with cell parameters a=0.83359(6) nm, b=1.09990(9) nm, c=0.75054(7) nm, α=91.412(3)°, β=96.683(3)°, γ=107.997(6)°, V=0.64869(9)nm3, Z=1, Dc=1.621Mg/m3, F(000)324, μ(Mo Kα)=1.374mm-1, R=0.0318 and wR=0.0864 for 2547 observed reflections, GOF=1.112. Complex 2 belongs to triclinic system, space group P1, a=0.69038(6) nm, b0.94607(9) nm, c=1.18582(7) nm, α=89.383(5)°, β=81.515(2)°, γ=69.214(2)°, V=0.7155(1)nm3, Z=2, Dc=1.704 Mg/m3, F(000)=370, μ(Mo Kα)=1.433 mm-1, R=0.0681 and wR=0.1352 for 1720 observed reflections, GOF=1.056. The binuclear complex 1 has a crystallographic center. The two methanol oxygen atoms in complex 1 bridges two iron atoms, forming a Fe2(μ-O)2core with crystallographic centrosymmetry and Fe...Fe distance is 0.31609 nm. The iron atom is octahedrally coordinated by two nitrogen atoms and one oxygen of the N-acetylpicoloylhydrazide ligand, two methanol oxygen atoms and one chloride ion. The neighboring molecules in complex 1 are connected by hydrogen bonding, forming an infinite chain structure. The iron(Ⅲ) ion in complex 2 has a strongly distorted square pyramidal geometry with three donors of the N-phenylpicoloylhydrazide ligand and two chloride ions. The two centrosymmetry-related molecules of complex 2 are connected as a pair by two N-H...Ohydrogen bonds. In the two title complexes, ν(C=O) and ν(C-N) are shifted to lower frequencies in IRspectra; π-π*charge transitions and d-π*charge-transitions are observed in their electronic spectra. The emission lines (λex=310 nm) are shifted to higher frequencies in fluorescence spectra. |
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| Keywords: | Crystal structure Picoloylhydrazide Iron complex |
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