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Pyrazolato Metal Complexes: Synthesis, Characterization and X-ray Crystal Structures of Rhenium(I) Derivatives

✍ Scribed by G. Attilio Ardizzoia; Girolamo LaMonica; Angelo Maspero; Massimo Moret; Norberto Masciocchi

Publisher: John Wiley and Sons
Year: 1998
Tongue: English
Weight: 408 KB
Volume: 1998
Category: Article
ISSN: 1434-1948
DOI: 10.1002/(sici)1099-0682(199810)1998:10<1503::aid-ejic1503>3.0.co;2-0

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✦ Synopsis

The mononuclear complexes [Re(CO) 3 (Hpz) 2 Br] (1) and [Re(CO) 3 (py)(Hpz)(pz)] species (6). The analogues of 4 and 6 with Hdmpz, i.e. [Re(CO) 3 (Hdmpz) 2 (dmpz)] ( ) and [Re(CO) 3 (Hdmpz) 2 Br] (2) were obtained by treating [Re(CO) 5 Br] with pyrazole (Hpz) or 3,5-dimethylpyrazole [Re(CO) 3 (py)(Hdmpz)(dmpz)] (8) were also synthesized. All species were characterized in solution by 1 H-NMR (Hdmpz). Complex 1 reacted with triethylamine affording a mixture of the ionic dinuclear derivative (Et 3 NH)[Re 2 -spectroscopy, while the crystal structures of complexes 1, 3, 4 and 6 were determined by single-crystal X-ray diffraction (CO) 6 (pz) 2 Br] (3) and of the mononuclear species [Re(CO) 3 -(Hpz) 2 (pz)] (4). Complex 4 was obtained in a pure form by analysis. The [(CO) 3 Re(µ-pz) 2 (µ-Br)Re(CO) 3 ] -anion represents the first structurally characterized species containing carrying out the reaction in the presence of excess free pyrazole. Treatment of 4 with pyridine afforded the rhenium(I) atoms bridged by µ-pyrazolate ligands.

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