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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 27, Number 11
BKCSDE 27(11)
November 20, 2006 

 
Title
Synthesis and Characterization of Dinuclear Ni(II) Complexes with Tetraazadiphenol Macrocycle Bearing Cyclohexanes
Author
Ki Ju Kim, Duk Sang Jung, Duk Soo Kim, Chi Kyu Choi, Ki Min Park, Jong Chul Byun*
Keywords
Tetraazadiphenolic macrocycle, Macrocyclic nickel(II) complex, Crystal structure, Isothiocyanato ligand
Abstract
The dinuclear tetraazadiphenol macrocyclic nickel(II) complexes [Ni2([20]-DCHDC)]Cl2 (I), [Ni2([20]-DCHDC)](ClO4)2·2CH3CN (II(b)) and [Ni2([20]-DCHDC)(NCS)2] (III) {H2[20]-DCHDC = 14,29-dimethyl-3,10,18,25-tetraazapentacyclo-[25,3,1,04,9,112,16,019,24]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 N2O2 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 [Ni2([20]-DCHDC)(Cl+ 2H)]+, [Ni2([20]-DCHDC)(ClO4 + 2H)]+ and [Ni2([20]-DCHDC)(NCS) + 6H]+, respectively.
Page
1747 - 1751
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