대한화학회지 (Journal of the Korean Chemical Society)

  • 제39권7호
  • /
  • Pages.552-558
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  • 1995
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  • 1017-2548(pISSN)
  • /
  • 2234-8530(eISSN)
대한화학회 (Korean Chemical Society)
권호 표지

부틸아미드옥심 유도체의 몰리브덴(Ⅵ) 사핵 착물의 합성과 성질

Synthesis and Characterization of Tetranuclear Molybdenum(Ⅵ) Complexes with Butylamidoxime Derivatives

  • 로수균 (경북대학교 자연과학대학 화학과) ;
  • 오상오 (경북대학교 자연과학대학 화학과)
  • Roh, Soo-Gyun (Department of Chemistry, Kyungpook National University) ;
  • Oh, Sang Oh (Department of Chemistry, Kyungpook National University)
  • 발행 : 19950700
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초록

배위자인 이소부틸, 노르말 부틸 및 메틸티오아세트아미드옥심과 출발 물질인 단핵 및 다핵 착물과의 반응에서 $X_2[M_{O4}O_12{R'C(NH_2)NO}_2](X=n-Bu_4N^+$, $R'=(CH_3)_2CH$, $CH_3CH_2CH_2$, $CH_3SCH_2$; $X=(CH_3)_2CHC(=NH_2)NH_2^+$, $R'=(CH_3)_2CH$; $X=CH_3CH_2CH_2C(=NH_2)NH_2^+$, $R'=CH_3_CH_2CH_2$; $X=CH_3SCH_2C(=NH_2)NH_2^+$, $R'=CH_3SCH_2)$을 합성하였다. 합성한 착물은 원소분석, 적외선 및 핵자기공명에 의해 구조를 규명하였다. 얻은 착물중 ${(CH_3)_2CHC(NH_2)_2}_2[M_{O4}O_{12}{(CH_3)_2CHC(NH_2)NO}_2]$은 X-선 단결정 회절에서 결정구조를 밝혔고, 얻은 데이타는 Monoclinic, $P2_{1/c}$, $a=10.168(3){\AA}$, $b=11.768(1){\AA}$, $c=13.557(1){\AA}$, ${\beta}=102.08(1)^{\circ}$, $V=1586.2(5){\AA}^3$, Z = 2이었고, 회절강도 2951개($F_0>3s(F_0)$)에 대한 최종 신뢰도 인자는 0.026이었다. 이 착물의 구조는 평면상의 환형$[Mo_4({\mu}-O)_4]$과 두 개의 ${\mu}_4$-아미드옥시메이트로 구성되어 있다.

The tetranuclear complexes, $X_2[M_{O4}O_12{R'C(NH_2)NO}_2](X= n-Bu_4N^+$, $R'=(CH_3)_2CH$, $CH_3CH_2CH_2$, $CH_3SCH_2$; $X=(CH_3)_2CHC(=NH_2)NH_2^+$, $R'=(CH_3)_2CH$; $X = CH_3CH_2CH_2C(=NH_2)NH_2^+$, $R'=CH_3_CH_2CH_2$; $X=CH_3SCH_2C(=NH_2)NH_2^+$, $R'=CH_3SCH_2)$ have been synthesized by the reactions of monomeric and polynuclear complexes with isobutyl-, butyl- and thiomethylacetamidoxime. The prepared complexes were identified by elemental analysis, infrared, $^1H$ NMR and $^{13}C$ NMR spectroscopy. The structure of complex ${(CH_3)_2CHC(NH_2)_2}_2[M_{O4}O_{12}{(CH_3)_2CHC(NH_2)NO}_2]$ was determined by X-ray single crystal diffraction. Crystal data are follows: Monoclinic, $P2_{1/c}$, $a=10.168(3){\AA}$, $b=11.768(1){\AA}$, $c=13.557(1){\AA}$, ${\beta}=102.08(1)^{\circ}$, $V=1586.2(5){\AA}^3$, Z=2, final R=0.026 for 2951($F_0>3s(F_0)$). This complex is composed of a planar cyclic $[Mo_4({\mu}-O)_4]$ and two ${\mu}_4$-amidoximate.

키워드

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