Pyrazolate thiocarbonylrhodium complexes. X-ray structure of [Rh(μ-3,5-Me2Pz)(CS)(PPh3)]2 |
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Authors: | R Usón LA Oro MA Ciriano D Carmona A Tiripicchio MTiripicchio Camellini |
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Institution: | Departamento de Quimica Inorgánica, Universidad de Zaragoza, Zaragoza Spain;Istituto di Chimica Generale ed Inorganica, Universitá di Parma, Centro di Studio per la Strutturistica Diffrattometrica del C.N.R., Via M. D''Azeglio 85, Parma Italy |
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Abstract: | The preparation and properties of complexes of general formulae Rh(CS)-(HL)(PR3)2]ClO4 (HL = pyrazole (HPz), 3-methylpyrazole (H3-MePz), 3,5-dimethylpyrazole (H3,5-Me2Pz), PR3 = triphenylphosphine, tricyclohexylphosphine) and (PR3)2(CS)Rh(μ-Pz)AuPPh3]ClO4 are reported. Complexes of the first set react with potassium hydroxide to give Rh(μ-L)(CS)(PPh3)2 or RhPz(CS)(PR3)2 complexes. The structure of the complex Rh(3,5-Me2Pz)(CS)(PPh3)]2 has been determined by X-ray diffraction methods. The crystals are monoclinic, space group P21/c, with Z = 4 in a unit cell of dimensions a = 12.700(11), b = 17.217(16), c = 23.041(18) Å, β = 116.55(8)°. The structure has been solved by Patterson and Fourier methods and refined by full-matrix least-squares to R = 0.059 for 1978 independent reflections. The structure consists of dimeric complexes, in which each rhodium atom is in a square-planar environment being bonded to a carbon atom of a thiocarbonyl ligand, a phosphorus atom of a triphenylphosphine molecule and to two nitrogen atoms of pyrazolate ligands bridging the metal atoms. The dihedral angle of 71.1° between such two square planes leads to a bent configuration with an intramolecular rhodium-rhodium distance of 3.220 Å. The thiocarbonyl and triphenylphosphine ligands are in a trans disposition. |
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Keywords: | Author to whom correspondence should be directed |
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