The molecular structures of thiomethoxymethylbis(triphenylphosphine)-palladium hexafluorophosphate and perchlorate at -160 .DEG.C.

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概要

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• The molecular structures of [Pd(CH<SUB>2</SUB>SCH<SUB>3</SUB>)(PPh<SUB>3</SUB>)<SUB>2</SUB>]PF<SUB>6</SUB>(<B>3a</B>) and [Pd(CH<SUB>2</SUB>SCH<SUB>3</SUB>)(PPh<SUB>3</SUB>)<SUB>2</SUB>]ClO<SUB>4</SUB>(3B) at −160°C were determined by means of X-ray diffraction. Crystals of both complexes belong to the monoclinic system: <B>3a</B>, <I>a</I>=11.535(2), <I>b</I>=17.990(4), <I>c</I>=17.754(2) Å and β=101.07(1)°, space group P2<SUB>1</SUB>/c with <I>Z</I>=4; <B>3b</B>·CH<SUB>2</SUB>Cl<SUB>2</SUB> solvate, <I>a</I>=11.496(5), <I>b</I>=20.872(9), <I>c</I>=15.056(6) Å and β=94.77(4)°, space group P2<SUB>1</SUB>/n with <I>Z</I>=4. Both structures were solved by the heavy atom method and refined by the least-squares procedure to <I>R</I>=0.141 for 3906 reflections and <I>R</I>=0.102 for 4595 reflections for <B>3a</B> and <B>3b</B> respectively. The geometry around the Pd atom in each complex is essentially planar. However, the coordination behavior of the CH<SUB>2</SUB>SCH<SUB>3</SUB> group in <B>3a</B> and in <B>3b</B> seems to be different. In <B>3a</B>, the CH<SUB>2</SUB>SCH<SUB>3</SUB> group is bonded to the Pd atom through the Pd–C σ-bond and the donation of the sulfur to the metal atom, forming a Pd–C–S three-membered ring [Pd–CH<SUB>2</SUB>=2.06(4), Pd–S=2.367(8), CH<SUB>2</SUB>–S=1.77(4) and S–CH<SUB>3</SUB>=1.78(4) Å]. On the other hand, the CH<SUB>2</SUB>SCH<SUB>3</SUB> group in <B>3b</B> is coordinated to the metal atom as a methylenemethylsulfonium ion, containing a C=S double bond[Pd–CH<SUB>2</SUB>=2.208(13), Pd–S=2.303(6), CH<SUB>2</SUB>–S=1.678(14) and S–CH<SUB>3</SUB>=1.86(4) Å].

• 公益社団法人 日本化学会の論文

著者

• Miki Kunio

  Department Of Chemistry Graduate School Of Science Kyoto University

• Kai Yasushi

  Department Of Applied Chemistry Faculty Of Engineering Osaka University

• Kasai Nobutami

  Department Of Applied Biological Science Tokyo University Of Science

• Yasuoka Noritake

  Department Of Life Science Faculty Of Science Himeji Institute Of Technology

• Miki Kunio

  Department of Applied Chemistry, Faculty of Engineering, Osaka University

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