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Synthesis and Crystal Structure of an Ion- pair Compound: [HL]_2[Ni(CN)_4]·4H_2O (L = 4-(2- Hydroxyphenyl)-1,5, 9-triazacyclododecan-2-one)
引用本文:LI Jian-Ronga,b XIE Ya-Bob CAI Li-Zhena GUO Guo-Conga② BU Xian-Heb② HUANG Jin-Shuna a.Synthesis and Crystal Structure of an Ion- pair Compound: [HL]_2[Ni(CN)_4]·4H_2O (L = 4-(2- Hydroxyphenyl)-1,5, 9-triazacyclododecan-2-one)[J].结构化学,2004(4).
作者姓名:LI Jian-Ronga  b XIE Ya-Bob CAI Li-Zhena GUO Guo-Conga② BU Xian-Heb② HUANG Jin-Shuna a
作者单位:LI Jian-Ronga,b XIE Ya-Bob CAI Li-Zhena GUO Guo-Conga② BU Xian-Heb② HUANG Jin-Shuna a (State Key Laboratory of Structural Chemistry,Fujian Institute of Research on the Structure of Matter,The Chinese Academy of Sciences,Fuzhou,Fujian 350002,China) b (Department of Chemistry,Nankai University,Tianjin 300071,China)
基金项目:theNationalNaturalScienceFoundationofChina(No.20001007,20131020),NaturalScienceFoundationoftheChineseAcademyofSciences(KJCX2-H3)andFujianprovince(2000F006)
摘    要:1INTRODUCTIONCyclicpolyamineshaveoriginatedagreatdealofinterestowingtotheirbiologicalactivity1~3]andalotofmetalcomplexeswithmacrocyclicpoly-amineligandssuchastriamine12]aneN4,tetra-aminecyclen,cyclam,pentaamine16]aneN5,theirderivativesandsoonhavebeens…


Synthesis and Crystal Structure of an Ion- pair Compound: [HL]_2[Ni(CN)_4]·4H_2O (L = 4-(2- Hydroxyphenyl)-1,5, 9-triazacyclododecan-2-one)
Abstract:An ion-pair compound, HL]2Ni(CN)4]4H2O 1 has been obtained as an unexpected product when we attempt to prepare a heterometallic cyano-bridged complex by the reaction of GdCl3nH2O, K2Ni(CN)4 and L (L=4-(2-hydroxyphenyl)-1,5,9-triazacyclododecan-2-one) in aqueous solution, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.380(1), b = 9.9637(8), c = 17.087(1) ? ?= 105.947(2)? V = 2026.6(3) ?, Rint = 0.0509, Z = 2, Dc = 1.297 g/cm3, C34H56O8N10Ni, Mr = 791.60, F(000) = 844, m(MoKa) = 0.538 mm1, S = 1.030, the final R = 0.0644 and wR = 0.1299 for 2023 observed reflections with I ≥ 2(I). The title compound 1 contains one anion of Ni(CN)4]2, two cations of HL]+ and four packing water molecules, which are held together by the NH···O and OH···O hydrogen bonds to form a three- dimensional framework.
Keywords:tetracyanonickelate anion  macrocyclic triamine cation  crystal structure
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