The crystalline adduct of formula (DPK.H)+[{ReOCl2(DPK.OH)}2Cl]- was prepared by the reaction of trans-ReOCl3(PPh3)2 with di-(2-pyridyl)ketone (DPK) in THF or dichloromethane. The compound was characterized by elemental analysis, vibrational, optical and H-1 NMR spectroscopy. The evidence suggests that the coordinated DPK ligands have undergone addition of water at the carbonylic carbon atom, and that the (C5H4N)2C(O)(OH) moiety acts as a uninegative, terdentate N,O,N-donor ligand. The X-ray crystal structure of the compound is also reported. Crystal data: C33H27Cl5N6O7Re2, triclinic, space group P1-; a = 9.483(3), b = 14.399(5), c = 15.413(7) angstrom, alpha = 110.68(3), beta = 104.73(3), gamma = 92.66(3)-degrees and U=1879.9(9) angstrom3 to give Z = 2 for D(calc) = 2.07 Mg/m3.
Nucleophilic addition of water to coordinated di-(2-pyridyl)ketone (DPK) in rhenium(V) complexes. Synthesis and crystal structure of the adduct (DPK·H)+[{ReOCl2(DPK·OH)}2Cl]−
BANDOLI, GIULIANO;DOLMELLA, ALESSANDRO;
1994
Abstract
The crystalline adduct of formula (DPK.H)+[{ReOCl2(DPK.OH)}2Cl]- was prepared by the reaction of trans-ReOCl3(PPh3)2 with di-(2-pyridyl)ketone (DPK) in THF or dichloromethane. The compound was characterized by elemental analysis, vibrational, optical and H-1 NMR spectroscopy. The evidence suggests that the coordinated DPK ligands have undergone addition of water at the carbonylic carbon atom, and that the (C5H4N)2C(O)(OH) moiety acts as a uninegative, terdentate N,O,N-donor ligand. The X-ray crystal structure of the compound is also reported. Crystal data: C33H27Cl5N6O7Re2, triclinic, space group P1-; a = 9.483(3), b = 14.399(5), c = 15.413(7) angstrom, alpha = 110.68(3), beta = 104.73(3), gamma = 92.66(3)-degrees and U=1879.9(9) angstrom3 to give Z = 2 for D(calc) = 2.07 Mg/m3.Pubblicazioni consigliate
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