Preparation and characterization of cis- and trans-(RhCl2(dmap)2)+ (dmap=1,3-bis(dimethylarsino)propane), and X-ray structure analyses of these complexes and trans-(CoCl2(dmap)2)+.

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• The <I>cis</I>- and <I>trans</I>- [RhCl<SUB>2</SUB>(dmap)<SUB>2</SUB>]<SUP>+</SUP> (dmap=1,3-bis(dimethylarsino)propane) complexes were prepared by reaction of RhCl<SUB>3</SUB>·3H<SUB>2</SUB>O with dmap, and the molecular structures of these complexes were determined by the single crystal X-ray diffraction method. Crystal data and final <I>R</I> values are: <I>trans</I>-[RhCl<SUB>2</SUB>(dmap)<SUB>2</SUB>]ClO<SUB>4</SUB> (<B>1</B>), monoclinic, Cc, <I>a</I>=20.018(4), <I>b</I>=10.229(1), <I>c</I>=12.972(2) Å, β=99.98(2)°, <I>V</I>=2616(1) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.034 for 1298 observed unique reflections. <I>cis</I>-[RhCl<SUB>2</SUB>(dmap)<SUB>2</SUB>]PF<SUB>6</SUB> (<B>2a</B>), orthorhombic, Pca2<SUB>1</SUB>, <I>a</I>=14.699(2), <I>b</I>=9.381(2), <I>c</I>=19.640(9) Å, <I>V</I>=2704(1) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.086 for 1284 reflections. cis-[RhCl<SUB>2</SUB>(dmap)<SUB>2</SUB>]CF<SUB>3</SUB>SO<SUB>3</SUB> (<B>2b</B>), orthorhombic, Pca2<SUB>1</SUB>, <I>a</I>=14.700(3), <I>b</I>=9.381(4), <I>c</I>=19.644(8) Å, <I>V</I>=2709(2) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.088 for 1094 reflections. The Rh–As distances in the linear As–Rh–As groups are 2.442(4)–2.454(4) Å (av 2.446(4) Å) for (<B>1</B>), 2.345(4) and 2.484(6) (av 2.415(6) Å) for (<B>2a</B>), and 2.389(10) and 2.441(10) Å (av 2.415(10) Å) for (<B>2b</B>), while those in the linear As–Rh–Cl groups are 2.385(3) and 2.370(4) Å (av 2.378(4) Å) for (<B>2a</B>), and 2.387(4) and 2.367(5) Å (av 2.377(5) Å) for (<B>2b</B>). The molecular structure of <I>trans</I>-[CoCl<SUB>2</SUB>(dmap)<SUB>2</SUB>]Clo<SUB>4</SUB> (<B>3</B>) was also determined by the X-ray method. Crystal data and the final <I>R</I> value are: orthorhombic, Pccm, <I>a</I>=8.018(2), <I>b</I>=8.428(1), <I>c</I>=18.716(3) Å, <I>V</I>=1265 Å<SUP>3</SUP>, <I>Z</I>=2, <I>R</I>=0.095 for 1072 reflections. A series of <I>trans</I>-[RhX<SUB>2</SUB>(dmap)<SUB>2</SUB>]<SUP>+</SUP> (X=Cl, Br, I) were prepared and their absorption spectra were compared with one another and with those of related complexes.

• 公益社団法人 日本化学会の論文

著者

• Kojima Masaaki

  Department Of Chemistry Faculty Of Science Okayama University

• Saito Yoshihiko

  Department Of Cardiology Juntendo University School Of Medicine

• OHBA SHIGERU

  Deparment of Biology, Faculty of Science, Tokyo Metropolitan University

• Fujita Junnosuke

  Department of Chemistry Faculty of Science Osaka University

• HAMADA Masatoshi

  Department of Applied Mathematics, Faculty of Engineering, Yokohama National University

• Saito Yoshihiko

  Department of Chemistry, Faculty of Science and Technology, Keio University

• Suzuki Nahomi

  Department of Chemistry, Faculty of Science and Technology, Keio University

• Simonsen Kim

  Chemistry Department I, H. C. Ørsted Institute, University of Copenhagen

• Galsbøl Frode

  Chemistry Department I, H. C. Ørsted Institute, University of Copenhagen

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