Studies of rhenium–carboxylate complexes. I. Tris(μ- i -butyrato)di(chlororhenium(III)) perrhenate
1969; NRC Research Press; Volume: 47; Issue: 22 Linguagem: Inglês
10.1139/v69-696
ISSN1480-3291
AutoresC. Calvo, N.C. Jayadevan, C. J. L. Lock,
Tópico(s)Synthetic Organic Chemistry Methods
ResumoOne of the compounds obtained by reacting rhenium(III) chloride with isobutyric acid while exposed to oxygen has been shown by single crystal X-ray diffraction to be tris(μ-i-butyrato)di(chlororhenium(III)) perrhenate. The crystals are monoclinic with lattice parameters a = 8.980(5) Å, b = 17.790(8) Å, c = 15.361(8) Å, and β = 114.4(1)°. The space group is P2 1 / c and there are 4 formula units per cell. A total of 1729 independent reflections were examined and the structure was refined by full three dimensional least squares to an R value of 0.114. Two Re environments are found, one consisting of a dimer unit bridged by three carboxylate groups with a chlorine atom per rhenium and the other as a perrhenate group. This latter group, showing a mean Re—O distance of 1.74 Å, shares an oxygen atom with a Re in the dimer unit, and this Re—O bond length is 2.28 Å long. The structure consists of a packing of chains of alternate dimers and perrhenate groups running parallel to the c axis.
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