Absorption, circular dichroism, and nuclear magnetic resonance studies of bis(acetylacetonato)cobalt(III) complexes containing 2-aminoalkylphosphine chelates with phosphorus and nitrogen donor atoms.

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概要

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• Bis(acetylacetonato)cobalt(III) complexes containing a variety of 2-aminoalkylphosphines, NH<SUB>2</SUB>CH<SUB>2</SUB>CH<SUB>2</SUB>P(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB>, (CH<SUB>3</SUB>)<SUB>2</SUB>NCH<SUB>2</SUB>CH<SUB>2</SUB>P(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB>, (<I>S</I>)-NH<SUB>2</SUB>CH(CH<SUB>3</SUB>)CH<SUB>2</SUB>P(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB>, <I>rac</I>-NH<SUB>2</SUB>CH<SUB>2</SUB>CH<SUB>2</SUB>P(CH<SUB>3</SUB>) (C<SUB>6</SUB>H<SUB>5</SUB>), (<I>R</I>)-NH<SUB>2</SUB>CH<SUB>2</SUB>CH<SUB>2</SUB>P(C<SUB>4</SUB>H<SUB>9</SUB>)(C<SUB>6</SUB>H<SUB>5</SUB>), and NH<SUB>2</SUB>CH<SUB>2</SUB>CH<SUB>2</SUB>P(CH<SUB>3</SUB>)<SUB>2</SUB>, and a diphosphine, (C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB>PCH<SUB>2</SUB>CH<SUB>2</SUB>P(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB> were prepared and resolved (or separated) into optical isomers by SP-Sephadex column chromatography. Absorption, circular dichroism, and <SUP>1</SUP>H and <SUP>13</SUP>C NMR spectra of the new complexes were measured and the results compared with those of the related complexes. Positions of the 2-aminoalkylphosphine and the related ligands in the spectrochemical series were as follows; CN<SUP>−</SUP>>NH<SUB>2</SUB>CH<SUB>2</SUB>CH<SUB>2</SUB>P(CH<SUB>3</SUB>)<SUB>2</SUB>>(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB>PCH<SUB>2</SUB>CH<SUB>2</SUB>P(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB>>NH<SUB>2</SUB>CH<SUB>2</SUB>CH<SUB>2</SUB>P(CH<SUB>3</SUB>) (C<SUB>6</SUB>H<SUB>5</SUB>)(<U>Remark: Graphics omitted.</U>)NH<SUB>2</SUB>CH<SUB>2</SUB>CH<SUB>2</SUB>P(C<SUB>4</SUB>H<SUB>9</SUB>)(C<SUB>6</SUB>H<SUB>5</SUB>)>NH<SUB>2</SUB>CH(CH<SUB>3</SUB>)CH<SUB>2</SUB>P(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB>(<U>Remark: Graphics omitted.</U>)NH<SUB>2</SUB>CH<SUB>2</SUB>CH<SUB>2</SUB>P(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB>(<U>Remark: Graphics omitted.</U>)NH<SUB>2</SUB>CH<SUB>2</SUB>CH<SUB>2</SUB>NH<SUB>2</SUB>>(CH<SUB>3</SUB>)<SUB>2</SUB>NCH<SUB>2</SUB>CH<SUB>2</SUB>P(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>2</SUB>. For the <SUP>13</SUP>C NMR spectra, all the signals including those due to two diastereotopic phenyl groups on a phosphorus atom were assigned, and the chemical shifts and the coupling constants were determined. The methyl and carbonyl carbons which are trans to a phosphorus atom give a doublet signal due to four-bond (<SUP>4</SUP><I>J</I>(C,P)=6–7 Hz) and three-bond (<SUP>3</SUP><I>J</I>(C,P)=2–3 Hz) couplings, respectively, through a cobalt(III) ion.

• 公益社団法人 日本化学会の論文

著者

• Ito Tasuku

  Institute For Molecular Science

• Kashiwabara Kazuo

  Department Of Chemistry Faculty Of Science Nagoya University

• Kinoshita Isamu

  Department Of Chemistry Graduate School Of Science Osaka City University

• Fujita Junnosuke

  Department of Chemistry Faculty of Science Osaka University

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