Synthesis and Crystal Structure of an Ion-Pair Compound:[HL]2[Ni(CN)4] 4H2O(L=4-(2-Hydroxyphenyl)-1,

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An ion-pair compound,[HL]2[Ni(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 GdCl3·nH2O,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)A,β=105.947(2)°,V=2026.6(3) A3,Rint=0.0509,Z=2,Dc=1.297g/cm3,C34H56O8N10Ni,Mr=791.60,F(000)=844,μ(MoKα)=0.538 mm-1,S=1.030,the final R=0.0644 and wR=0.1299 for 2023 observed reflections with I≥2σ(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 N-H…O and O-H…O hydrogen bonds to form a three-dimensional framework.
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