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Synthesis and Crystal Structure of a New N-alkylated Azacrown Ligand

Synthesis and Crystal Structure of a New N-alkylated Azacrown Ligand
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摘要 A new pendant arms macrocyclic ligand, N, N'-bis(2-cyanoethyl)-3,4: 9, 10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane (L), was synthesized in goodyield (93% ) by alkylating 3, 4: 9, 10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane(L') with acrylonitrile. Its crystal structure has been determined by X-ray diffraction.The ligand crystallizes in the orthorhombic system, space group Pbca, a=18. 143 (3),b=11. 206(2), c=22. 274(5)A, V=4528(2)A3, Mr=418. 55, Z= 8, F(000)=1792, Dc= 1. 228 gcm-3, T= 293K, μ= 7. 9 cm-1, final R=0.044 and Rw=0.067(w=1/(σ2 (F) + 0. 0005F2 ) ) based on 2291 independent reflections with F> 4. 0σ(F). The two benzene rings of the macrocyclic ligand are not in the same plane, andthe dihedral angle between them is 73. 6°, the molecule is in a folded state. A new pendant arms macrocyclic ligand, N, N'-bis(2-cyanoethyl)-3,4: 9, 10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane (L), was synthesized in goodyield (93% ) by alkylating 3, 4: 9, 10-dibenzo-1, 12-diaza-5, 8-dioxacyclopentadecane(L') with acrylonitrile. Its crystal structure has been determined by X-ray diffraction.The ligand crystallizes in the orthorhombic system, space group Pbca, a=18. 143 (3),b=11. 206(2), c=22. 274(5)A, V=4528(2)A3, Mr=418. 55, Z= 8, F(000)=1792, Dc= 1. 228 gcm-3, T= 293K, μ= 7. 9 cm-1, final R=0.044 and Rw=0.067(w=1/(σ2 (F) + 0. 0005F2 ) ) based on 2291 independent reflections with F> 4. 0σ(F). The two benzene rings of the macrocyclic ligand are not in the same plane, andthe dihedral angle between them is 73. 6°, the molecule is in a folded state.
出处 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1997年第3期195-199,共5页 结构化学(英文)
关键词 SYNTHESIS crystal structure N-alkylated ligand AZACROWN synthesis, crystal structure, N-alkylated ligand, azacrown
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参考文献15

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