Synthesis and structural analysis of new palladium(II) thiosaccharinates with triphenylphosphane or diphosphanes, Susana H. Tarulli, Oscar V. Quinzani, Sandra D. Mandolesi, Jorge A. Guida, Gustavo A. Echeverría, Oscar E. Piro and Eduardo E. Castellano, Ze

SUSANA H. TARULLI, OSCAR V. QUINZANI, SANDRA D. MANDOLESI, JORGE A. GUIDA, GUSTAVO A. ECHEVERRÍA, OSCAR E. PIRO AND EDUARDO E. CASTELLANO

ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE

Wiley Interscience

Año: 2009 vol. 635 p. 1604 - 1612

0044-2313

AbstractA series of palladium(II) thiosaccharinates with triphenylphosphane (PPh3),bis(diphenylphosphino)methane (dppm), and bis(diphenylphosphino)ethane (dppe) havebeen prepared and characterized. From mixtures of thiosaccharin, Htsac, andpalladium(II) acetylacetonate, Pd(acac)2, the palladium(II) thiosaccharinate, Pd(tsac)2(tsac: thiosaccharinate anion) (1) was prepared. The reaction of 1 with PPh3, dppm, anddppe leads to the mononuclear species Pd(tsac)2(PPh3)2·MeCN (2), [Pd(tsac)2(dppm)](3), Pd(tsac)2(dppm)2 (4), and [Pd(tsac)2(dppe)]·MeCN (5). Compounds 2, 4, and 5 havebeen prepared also by the reaction of Pd(acac)2 with the corresponding phosphane andHtsac. All the new complexes have been characterized by chemical analysis, UVvisible,IR and Raman spectroscopy. Some of them have been also characterized byNMR spectroscopy. The crystalline structures of complexes 3, and 5 have been studiedby X-ray diffraction techniques. Complex 3 crystallizes in the monoclinic P21/n spacegroup with a=16.3537(2), b=13.3981(3), c=35.2277(7) Å, β=91.284(1)°, and Z=8molecules per unit cell, and 5 in P21/n with a=10.6445(8), b=26.412(3), c=15.781(2) Å,