Journal of the Korean Chemical Society (대한화학회지)

Korean Chemical Society (대한화학회)
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Metal-Nitrosyl Complexes(II) : Synthesis and Characterization of Dinitrosyltungsten(O) Complexes

금속-니트로실 착물 (제 2 보) : 디니트로실 텅스텐(O) 착물의 합성과 특성

  • Sang-Oh Oh (Department of Chemistry, College of Natural Science, Kyungpook National University) ;
  • Seong-Jong Mo (Department of Chemistry, College of Natural Science, Kyungpook National University)
  • 오상오 (경북대학교 자연과학대학 화학과) ;
  • 모성종 (경북대학교 자연과학대학 화학과)
  • Published : 1992.12.20
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Abstract

The polymeric compound [{$W(NO)_2Cl_2$}$_n$] were prepared by reductive nitrosylation of $WNaNO_2$ and acidified $WFeSO_4$ with $WWCl_6$ at room temperature. The reactions of [{$W(NO)_2Cl_2$}$_n$] with unidentate and bidentate ligands afforded neutral monomeric [$W(NO)_2Cl_2L_2$(or L-L)] in a relative high yields (70$\sim$90%). 3,5-lutidine, ${\gamma}$-cyanopyridine, 1,2-phenylenediamine, 1,10-phenanthroline, sym-diphenylethylenediamine, 9,10-phenanthrenequinone, 1,3-bis(diphenylphosphino)propane, 1,1'-bis(diphenylphosphino)ferrocene and 8-hydroxyquinoline were used as coordinating ligands. These dinitrosyltungsten complexes were characterized by elemental analysis, $^1H$-NMR, infrared, and UV-visible spectroscopy are reported. The spectral data indicated that geometric structures of the products were cis-dinitrosyl-trans-dichloro-cis-$L_2$ of $C_{2v}$ symmetry.

실온에서 $WCl_6$와 $WNaNO_2$ 및 산성화시킨 $WFeSO_4$의 환원성 니트로실화 반응을 통해 다핵 화합물인 [{$W(NO)_2Cl_2$}$_n$]을 합성하였다. 이 [{$W(NO)_2Cl_2$}$_n$]와 한자리 및 두자리 리간드를 반응시켜 비교적 높은 수득률(70$\sim$90%)로 중성의 단핵 화합물인 [$W(NO)_2Cl_2L_2$(or L-L)]을 얻었다. 배위 리간드로는 3,5-lutidine, ${\gamma}$-cyanopyridine, 1,2-phenylenediamine, 1,10-phenanthroline, sym-diphenylethylenediamine, 9,10-phenanthrenequinone, 1,3-bis(diphenylphosphino)propane, 1,1'-bis(diphenylphosphino)ferrocene 및 8-hydroxyquinoline을 사용하였다. 합성한 디니트로실텡스텐 착물은 원소분석과 적외선, 핵자기 공명 및 전자 흡수 스펙트럼 등을 이용해서 그 특성을 조사하였으며 이들 분광학적 결과로써 모든 화합물의 기하학적 구조가 $C_{2v}$ 대칭인 cis-dinitrosyl-trans-dichloro-cis-$L_2$의 구조임을 확인하였다.

Keywords

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