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Structure and NMR Spectroscopy in Solid State and Solution of {Na2[μ2-(C6H4O2)2](C6H4OOH)2}^4-

Structure and NMR Spectroscopy in Solid State and Solution of {Na2[μ2-(C6H4O2)2](C6H4OOH)2}^4-
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摘要 The new compound (NH3CH2CH2NH3)2{Na2[μ2-(C6H4O2)2](C6H4OOH)2} has been synthesized and characterized by elemental analysis, IR, UV, NMR and single crystal X-ray diffraction. The yellow crystals crystallized in the triclinic system with space group P-1 and a=0.6091(2) nm, b= 1.0274(3) nm, c= 1.2466(4) nm, α=89.073(6)°, β=89.376(6)°, γ=78.873(5)°, V=0.7653(4) nm^3, Z= 1, R1=0.0568, wR2=0.1198. Every sodium ion coordinates in trigonal prismatic fashion with two O atoms from a terminal chelating catecholato ligand and four O atoms from bridging P2 catecholato ligands, Two neighboring NaO6 trigonal prisms are face-shared and centrosymmetric with regard to the inversion center consisting of four tri-bridging O atoms to form a binuclear cluster {Na2[μ2-(C6H4O2)2]}^2- anion. The comparison of ^13C NMR spectrum of tlie complex in solid state with that in solution indicated that the rapid exchange between the bridging [μ2-(C6H4O2]^2- and terminal [C6H4OOH]^- ligands was present in solution. The new compound (NH3CH2CH2NH3)2{Na2[μ2-(C6H4O2)2](C6H4OOH)2} has been synthesized and characterized by elemental analysis, IR, UV, NMR and single crystal X-ray diffraction. The yellow crystals crystallized in the triclinic system with space group P-1 and a=0.6091(2) nm, b= 1.0274(3) nm, c= 1.2466(4) nm, α=89.073(6)°, β=89.376(6)°, γ=78.873(5)°, V=0.7653(4) nm^3, Z= 1, R1=0.0568, wR2=0.1198. Every sodium ion coordinates in trigonal prismatic fashion with two O atoms from a terminal chelating catecholato ligand and four O atoms from bridging P2 catecholato ligands, Two neighboring NaO6 trigonal prisms are face-shared and centrosymmetric with regard to the inversion center consisting of four tri-bridging O atoms to form a binuclear cluster {Na2[μ2-(C6H4O2)2]}^2- anion. The comparison of ^13C NMR spectrum of tlie complex in solid state with that in solution indicated that the rapid exchange between the bridging [μ2-(C6H4O2]^2- and terminal [C6H4OOH]^- ligands was present in solution.
出处 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2006年第3期336-340,共5页 中国化学(英文版)
基金 Project supported by the National Natural Science Foundation of China (No. 20271034) and the Natural Science Foundation of Beijing City, China (No. 2012005).
关键词 sodium complex 1 2-dihydroxybenzene SYNTHESIS crystal structure sodium complex, 1,2-dihydroxybenzene, synthesis, crystal structure
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