Journal of the Korean Chemical Society (대한화학회지)

Korean Chemical Society (대한화학회)
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Metal-Dinitrosyl Complexes(Ⅳ) : Synthesis and Characterization of Symmetric and Asymmetric Dinuclear Molybdenum and Tungsten Complexes

금속-디니트로실 착물 (제 4 보) : 몰리브덴과 텅스텐의 대칭 및 비대칭 이핵 착물의 합성과 특성

  • 오상오 (경북대학교 자연과학대학 화학과) ;
  • 모성종 (경북대학교 자연과학대학 화학과)
  • Published : 19940700
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Abstract

Several new symmetric and asymmetric homo and hetero dinuclear complexes of the type $[Cl(dppp)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$ and $[Cl(phen)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$(M,M'= Mo or W; phen = 1,10-phenanthroline; dppp = 1,3-bis(diphenylphosphino)propane; pyz = 1,4-pyrazine) were synthesized in three-steps starting from $[M(NO)_2Cl_2]_n(M = Mo, W)$. The final products were purified by eluting it through silica gel column ($2{\times}20$ cm) with acetone as the eluent. Characterization of these complexes and some related complexes was accomplished through UV-vis., $^1H$-NMR, $^{13}C$-NMR and IR spectroscopies as well as elemental analysis. The infrared spectra indicate that the NO groups occupy cis-positions of the octahedral. The $^1H$ and $^{13}C-NMR$ data for the new compounds revealed a dimeric structures with bridged pyz.

$[M(NO)_2Cl_2]_n(M = Mo, W)$을 출발물질로 사용하여 3단계 합성과정을 거쳐 $[Cl(dppp)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$와 $[Cl(phen)(NO)_2M({\mu}-pyz)M'(NO)_2(dppp)Cl][ClO_4]_2$(M,M'= Mo or W; phen = 1,10-phenanthroline; dppp = 1,3-bis(diphenylphosphino)propane; pyz = 1,4-pyrazine) 형의 새로운 대칭 및 비대칭 이핵 착물을 합성하였다. 최종 생성물은 실리카겔 칼럼($2{\times}20$ cm)을 통해 아세톤으로 용리시켜 분리하였다. 합성한 착물은 원소분석과 적외선, 핵사기 공명 및 전자 흡수스펙트럼 등을 이용해서 그 특성을 조사하였다. 적외선 스펙트럼은 모든 착물이 팔면체 구조로서 두 개의 NO기가 cis 위치로 배위되어 있음을 나타냈으며, $^1H$ 및 $^{13}C$ 핵자기 공명 스펙트럼은 이들 착물이 pyz가 다리결합하고 있는 이핵 착물임을 나타내었다.

Keywords

References

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