Synthesis and Characterization of Dinuclear Mo(Ⅲ) and V(Ⅲ) Complexes (Ⅴ)

몰리브덴(Ⅲ)과 바나듐(Ⅲ) 이핵 착물의 합성과 특성 (제5보)

  • Oh, Sang-Oh (Department of Chemistry, Kyungpook National University) ;
  • Lyou, Eun-Young (Department of Chemistry, Kyungpook National University)
  • 오상오 (경북대학교 자연과학대학 화학과) ;
  • 류은영 (경북대학교 자연과학대학 화학과)
  • Published : 19950700

Abstract

The neutral complexes $MCl_3(phda)(MeCN)]$ and $[MCl_3(PPh_3)_2(MeCN)]$ (M=Mo, V) were prepared by the reaction of $MCl_z$, (M=Mo; z=5, M=V; z=3) with N, P-donating ligands in acetonitrile solution. Addition of AgClO_4$ to these neutral monomeric complexes in acetone solution afforded $MCl_{3-n}L_2(MeCN)(S)_n](ClO_4)_n$ (n=1, 2 : s=solvent). Two types of asymmetrical homo- and hetero-dinuclear complexes have been synthesized. The type of chloride bridged dinuclear complex is $[(MeCN)(phda)ClM({\mu}-Cl)_2M'Cl(PPh_3)_2(MeCN)](ClO_4)_2.$ And the type of pyrazine bridged complex is $[(MeCN)(phda)Cl_2M({\mu}-pyz)M'Cl_2(PPh_3)_2(MeCN)](ClO_4)_2.$ These complexes were characterized by elemental analysis, $^1H,\;^13C$ NMR, IR, Far-IR and UV-Vis spectroscopy.

$MCl_z(M=Mo;\;z=5,\;M=V;\;z=3)$과 N, P 주개 리간드를 acetonitrile 용매에서 반응시켜 중성 착물 $MCl_3(phda)(MeCN)]과 \; [MCl_3(PPh_3)_2(MeCN)](M=Mo,\;V)$을 합성하였다. Acetone 용액에서 이들 중성 착물과 AgClO_4$를 반응시켜 양이온 착물 $MCl_{3-n}L_2(MeCN)(S)_n](ClO_4)_n$(n=1,2:s=solvent)을 얻었다. 염소가 연결된 $[(MeCN)(phda)ClM({\mu}-Cl)_2M'Cl(PPh_3)_2(MeCN)](ClO_4)_2$ 및 pyrazine이 연결된 $[(MeCN)(phda)Cl_2M({\mu}-pyz)M'Cl_2(PPh_3)_2(MeCN)](ClO_4)_2$형의 호모(M=M'), 헤테로 $(M{\neq}M')$ 이핵 착물을 합성하였다. 합성한 착물들은 원소분석과 적외선, $^1H,\;^13C$ 핵자기 공명 및 전자 흡수스펙트럼을 이용하여 그 특성을 조사하였다.

Keywords

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