| 三维多孔配位聚合物{[Zn2(mal)2(4,4'-bipy)(H2O)2]•2(H2O)0.25}∞ (mal＝丙二酸根)的合成、结构及性质研究 |
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| 引用本文： | 曹向前,陈金香,陈阳,李红喜,任志刚,张勇,郎建平. 三维多孔配位聚合物{[Zn2(mal)2(4,4'-bipy)(H2O)2]•2(H2O)0.25}∞ (mal＝丙二酸根)的合成、结构及性质研究[J]. 化学学报, 2006, 64(24): 2496-2500 |
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| 作者姓名： | 曹向前 陈金香 陈阳 李红喜 任志刚 张勇 郎建平 |
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| 作者单位： | 曹向前（苏州大学化学化工学院,江苏省有机合成重点实验室,苏州,215123）;陈金香（苏州大学化学化工学院,江苏省有机合成重点实验室,苏州,215123）;陈阳（苏州大学化学化工学院,江苏省有机合成重点实验室,苏州,215123）;李红喜（苏州大学化学化工学院,江苏省有机合成重点实验室,苏州,215123）;任志刚（苏州大学化学化工学院,江苏省有机合成重点实验室,苏州,215123）;张勇（苏州大学化学化工学院,江苏省有机合成重点实验室,苏州,215123）;郎建平（苏州大学化学化工学院,江苏省有机合成重点实验室,苏州,215123;中国科学院上海有机化学研究所,金属有机化学国家重点实验室,上海,200035） |
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| 基金项目： | 国家自然科学基金（No.20525101）、江苏省自然科学研究基金（No.KB2004205）及中国科学院上海有机化学研究所金属有机化学国家重点实验室（No.06-26）资助项目. |
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| 摘 要： | ZnO, 丙二酸及4,4'-bipy按物质的量之比1∶3∶0.3溶于H2O和DMF混合溶剂中(体积比4∶1), 形成的无色溶液在50 ℃反应 3 d, 得到了标题化合物{[Zn2(mal)2(4,4'-bipy)(H2O)2]•2(H2O)0.25}∞ (mal＝丙二酸根), 对其进行了元素分析、红外光谱和X射线衍射表征, 测定了晶体结构. 该聚合物属单斜晶系, P21/n空间群, a＝0.71215(16) nm, b＝1.8685(4) nm, c＝0.73890(17) nm, β＝91.486(5)°, V＝0.9829(4) nm3, Z＝4, Dc＝1.811 g/cm3, Mr＝268.03, F(000)＝542, μ＝25.02 cm－1. 最终偏离因子R1＝0.0499, wR2＝0.1374. 该化合物中Zn原子和三个丙二酸根中的4个O原子、一个水分子和4,4'-bipy的一个N原子配位, 形成的ZnNO5八面体通过4,4'-bipy和丙二酸根桥联, 组成一种新颖的三维多孔结构, 其孔道中充填游离水分子. 此外还研究了该聚合物的热性质.
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| 关 键 词： | 锌配合物 丙二酸根 4,4'-联吡啶 晶体结构 合成 聚合物 |
| 收稿时间： | 2006-06-05 |
| 修稿时间： | 2006-09-14 |
Synthesis, Crystal Structure and Properties of a 3D Porous Coordination Polymer {[Zn2(mal)2(4,4'-bipy)(H2O)2]• 2(H2O)0.25}∞ (mal＝malonate) |
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| CAO,Xiang-Qiana CHEN,Jin-Xianga CHEN,Yanga LI,Hong-Xia REN,Zhi-Ganga ZHANG,Yonga LANG,Jian-Ping,a,b. Synthesis, Crystal Structure and Properties of a 3D Porous Coordination Polymer {[Zn2(mal)2(4,4'-bipy)(H2O)2]• 2(H2O)0.25}∞ (mal＝malonate)[J]. Acta Chimica Sinica, 2006, 64(24): 2496-2500 |
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| Authors: | CAO Xiang-Qiana CHEN Jin-Xianga CHEN Yanga LI Hong-Xia REN Zhi-Ganga ZHANG Yonga LANG Jian-Ping a b |
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| Affiliation: | (Key Laboratory of Organic Synthesis of Jiangsu Province, School of Chemistry and Chemical Engineering, Suzhou University, Suzhou 215123)(State Key Laboratory of Organometallic Chemistry, Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai 200032) |
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| Abstract: | Reaction of ZnO, malonic acid, 4,4'-bipy (molar ratio is 1∶3∶0.3) in H2O/DMF (V∶V＝4∶1) at 50 ℃ for 3 d gave the title compound {[Zn2(mal)2(4,4'-bipy)(H2O)2]•2(H2O)0.25}∞ (mal＝malonate). The compound was characterized by elemental analysis, IR spectrum and single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n with a＝0.71215(16) nm, b＝1.8685(4) nm, c＝0.73890(17) nm, β＝91.486(5)°, V＝0.9829(4) nm3, Z＝4, Dc＝1.811 g/cm3, Mr＝268.03, F(000)＝542, μ＝25.02 cm－1, R1＝0.0499 and wR2＝0.1374. The X-ray analysis revealed that the central Zn atom is octahedrally coordinated by four O atoms from three mal ligands, one O atom from H2O and one N atom from 4,4'-bipy. The resulting ZnNO5 octahedron is bridged by 4,4'-bipy and malonate ligands, forming a novel 3D porous structure with its channels filled with water molecules. In addition, the thermal properties of the polymeric compound were also investigated. |
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| Keywords: | zinc complex malonate 4 4'-bipyridine synthesis coordination polymer crystal structure |
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