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변종철,한성빈,정덕상,임희정,한충훈 濟州大學校 師範大學 科學敎育硏究所 1995 科學敎育 Vol.12 No.1
rac-5.5.7.12.12.14-hexamethy1-1,4,8,11-tetraazacyclotetradecane hydrate : Lm·H_(2)O was prepared and separated from the corresponding meso-isomer dihydrate according to the Curtis method. The racisomer was confirmed by spectroscopic data of NMR and IR spectroscopy. To synthesize the [CrL_m(OH)₂] complex. the racemic compound purified from meso and racemic mixture was reacted with Cr(II1) salt. The complx ion species {[SrL_m(OH)_(2)]^(+): λ_(max) = 613.0(ε_(max) = 116 M^(-1)cm^(-1)), {[CrLm(OH)(H_(2)O)]^(2+) : λ_(max) = 575.0nm(ε_(max) = 133M^(-1)cm^(-1)). [CrLm(H_(2)O)_(2)]^(3+) : λ_(max) = 532.0nm (ε_(max) = 172M^(-1)cm^(-1))} obtained from pH change of [CrLm(OH)_(2)(OH)_(3)]^(+) solution were confirmed from an electron absorption spectra. The result of the distribution diagram of chemical species proves that main products in the range of solution pH ≤ 3.5 . 3.5 <pH <7, and pH ≥ 7. are [CrLm(H_(2)O)_(2)]^(3+). [CrL_(m)(OH) (H_(2)O)^(2+). and [CrL_m(OH)_(2), respectively. At P~ 2.0, we synthesized several Cr(III)-macrocyclic complexes containing various axial ligands (L_(a) : I, Br^(-), CI^(-), S_(2)O_(3)^(2-), F^(-), malonate, NCS^-, oxalate) instead of H_(2)O. [CrL_m(OH_(2))]^(3+) + L_(a) →[CrL_(m)(L_(a))_(n)]^(+)(n = 1 or 2) Cr(III)-macrocyclic complexes combined with vaious ligands on the axial position were primarily confirmed with the mass spectrum. Especially, when the axial ligands are malonate, oxalate, and S_(2)O_(3)^(2-), a possible thermal decomposition reaction and redox potential are considered as follows: ◁표삽입▷(본문을 참조하세요) As well, a spectrochemical series was drawn up on the basis of the ligand field strength obtained from electron absorption spertra of the complexes, [CrL_(m)(La)_(n)]^(p+) F^(-), CI^(-) ~Br^(-)<I^(-)<S_(2)O_(3)^(2-)<OH^(-)<H_(2)O<mal~NCS^(-) We can expect that there is three d-d transition d^(3) ion Tanabe-Sugano diagram. ◁표삽입▷(본문을 참조하세요) However, we found only two trasitions because the other transition {^(4)A_(2)_g(F)→^(4)T_lg(P) : v_(3)} is obscured by absorption arising from charge transfer transition. ◁표삽입▷(본문을 참조하세요)