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The dinuclear tetraazadiphenol macrocyclic nickel(II) complexes [Ni 2 ([20]-DCHDC)]Cl 2 (I), [Ni 2 ([20]-DCHDC)](ClO 4 ) 2 ·2CH 3 CN (II(b)) and [Ni2([20]-DCHDC)(NCS)2] (III) {H 2 [20]-DCHDC = 14,29-dimethyl-3,10,18,25-tetraazapentacyclo-[25,3,1,0 4,9 ,1 12,16 ,0 19,24 ]ditriacontane-2,10,12,14,16(32),17,27(31), 28,30-decane-31,32-diol} have been synthesized by self-assembly and characterized by elemental analyses, conductances, FT-IR and FAB-MS spectra, and single crystal X-ray diffraction. The crystal structure of II(b) is determined. It crystallizes in the monoclinic space group P2(1)/c. The coordination geometries around Ni(II) ions in I and II(b) are identical and square planes. In complex III each Ni(II) ion is coordinated to N 2 O 2 plane from the macrocycle and N atoms of NCS - ions occupying the axial positions, forming a square pyramidal geometry. The nonbonded Ni···Ni intermetallic separation in the complex II(b) is 2.8078(10) A. The FAB mass spectra of I, II and III display major fragments at m/z 635.1, 699.4 and 662.4 corresponding to [Ni 2 ([20]-DCHDC)(Cl +2H)] + , [Ni2([20]-DCHDC)(C104 + 2H)] + and [Ni 2 ([20]-DCHDC)(NCS) + 6H] + , respectively.

Synthesis and Characterization of Dinuclear Ni(II) Complexes with Tetraazadiphenol Macrocycle Bearing Cyclohexanes