N-对R苯基氮杂15冠5八钼多酸钠超分子配合物的合成与结构 |
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引用本文: | 鲁晓明,刘顺诚,刘育,卜显和,洪少良.N-对R苯基氮杂15冠5八钼多酸钠超分子配合物的合成与结构[J].化学学报,1997,55(10):1009-1018. |
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作者姓名: | 鲁晓明 刘顺诚 刘育 卜显和 洪少良 |
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作者单位: | [1]首都师范大学化学系 [2]南开大学化学系 |
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摘 要: | 为研究大环化合物对客体分子的选择性, 合成了通式为NaL(Et2O)]2Na2Mo8O26的三种新型N-对R苯基氮杂15冠5八钼多酸钠超分子配合物(其中L分别为: N-苯基氮杂15冠5、N-对氯苯基氮杂15冠5和N-对甲苯基氮杂15冠5), 进行了元素分析, 红外光谱与核磁共振等结构参数的表征, 对R基为CH3的标题配合物作了X射线四圆衍射测定, 该晶体属单斜晶系, 空间群为P21/a,a=1.4590(4)nm, b=1.3817(3)nm, c=1.7639(5)nm, β=112.67(2)°, V=3.281(1)nm^3, Mr=2021.3, Dc=2.11g/cm^3,μ=2.37mm^-^1, F(000)=2048, R=0.045和Rw=0.057, 与Na.(DB18C6)(CH3OH)M6O19和Na(DB24C8)]2M6O19进行比较,结果表明: 大环化合物不仅对客体金属离子有分子识别性, 而且对与之抗衡的多酸阴离子也具有影响。
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关 键 词: | 红外分光光度法 元素分析 晶体结构 核磁共振谱法 氮杂环化合物 冠醚 |
Synthesis and crystal structure of {Na[N-(p-RPh)15C5](Et2O)}2Na2Mo8O26 |
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Abstract: | Three new supermolecular complexes of {NaN-(p-RPh)15C5](Et2O)}2Na2Mo8O26 (R=H, Cl, CH3) were synthesized by reaction of N-(para-substituted phenyl)-aza-15-crown-5 with (n-Bu)4N]4Mo8O26 and Na^+ in mixed solvent of CH3OH and CH3CN and crystallized in Et2O. The supermolecular complexes were characterized by C/H analysis, IR, and 1H NMR spectra and X-ray structure determination of {NaN-(p-CH3Ph)15C5](Et2O)}2Na2Mo8O26. This crown ether octamolybdate is monoclinic, space group P21/a, a=1.4590(4)nm, b=1.3817(3)nm, c=1.7639(5)nm, β =112.67(2)°, V=3.281(1)nm^3, Mr=2021.3, Dc=2.11g/cm^3, μ=2.37mm^-^1, F(000)=2048, R=0.045 and Rw=0.057. Comparison with Na.(DB18C6)(CH3OH)M6O19 and Na(DB24C8)]2M6O19 (M=W and Mo), it was indicated that the host crown ether compounds could not only recongnize the guest-metal cations, but also choose counterion anions of polymolybdates with defferent degree of polymerization to combine into the crystals. |
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Keywords: | INFRARED SPECTROPHOTOMETRY ELEMENTAL ANALYSIS CRYSTAL STRUCTURE NMR SPECTROMETRY NITROGEN HETEROCYCLICS CROWN ETHER |
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