X-Ray structures of di-.MU.-oxo, .MU.-oxo-.MU.-thio-, and di-.MU.-thio-.MU.-((R)-propylenediaminetetraacetato)-bis(oxomolybdate(V)) ions.

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概要

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• The crystal structures of Na<SUB>2</SUB>[Mo<SUB>2</SUB>O<SUB>4</SUB>(<I>R</I>-pdta)]·3H<SUB>2</SUB>O (<B>1</B>), Na<SUB>2</SUB>[Mo<SUB>2</SUB>O<SUB>3</SUB>S(<I>R</I>-pdta)]·4H<SUB>2</SUB>O (<B>2</B>), and Na<SUB>2</SUB>[Mo<SUB>2</SUB>O<SUB>2</SUB>S<SUB>2</SUB>(<I>R</I>-pdta)]·4H<SUB>2</SUB>O (<B>3</B>) have been determined from difTractometer data collected by the use of Mo <I>K</I>α radiation. The structures of <B>1</B>, <B>2</B>, and <B>3</B> were refined by the least-squares method to <I>R</I> 0.064, 0.040, and 0.058 for 1370, 2794, and 2141 nonzero reflections respectively. Each Mo<SUP>v</SUP> ion has a distorted octahedral coordination, and the two coordination octahedra share a common edge to form a binuclear complex. Two terminal oxo ligands are <I>cis</I> to the bridging oxide or sulfide. The <I>R</I>-pdta<SUP>4−</SUP> ligand bridges two Mo<SUP>v</SUP> ions, yielding a Mo–N–CH<SUB>2</SUB>–CH(CH<SUB>3</SUB>)–N–Mo ring with an equatorial methyl group, the N and carboxyl O atoms occupying the axial (<I>trans</I> to the terminal O) and equatorial positions respectively. A specific distortion of the donor-atom disposition is observed, which is represented as the twist (<I>Δ</I>) of the terminal O–O edges in the (<U>Remark: Graphics omitted.</U>) portion about the axis passing through the mid-points of the O–O edges (<I>Δ</I> denotes the absolute disposition of two skew edges or bonds), and as the twist (<I>Δ</I>) of Mo–N bonds about the Mo–Mo axis. The O=Mo bonds of the O=Mo–Mo=O segment in <B>1</B> twist in <I>Δ</I>, but those in <B>2</B> and <B>3</B> are virtually parallel. The distortion of donor-atom disposition is discussed on the basis of the strain due to chelate-ring formation.

• 公益社団法人 日本化学会の論文

著者

• Sasaki Yoichi

  Department Of Chemistry Faculty Of Science Hokkaido University

• Saito Kazuo

  Department Chemistry Faculty Of Science Tohoku University

• Kuroya Hisao

  Department of Chemistry, Okayama University of Science

• Kojima Akinobu

  Department of Chemistry, Faculty of Science, Osaka City University

• Suzuki Kimiko

  Department of Chemistry, Faculty of Science, Tohoku University

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