TY - JOUR
T1 - Preparation, NMR studies and crystal structure of mononuclear and dinuclear Pd(II) and Pt(II) complexes that contain 1,2-bis[3-(3,5-dimethyl-1-pyrazolyl)-2-thiapropyl]benzene
AU - de León, Antonio
AU - Pons, Josefina
AU - García-Antón, Jordi
AU - Solans Huget, Xavier
AU - Font-Bardia, Mercè
AU - Ros, Josep
PY - 2007/8/6
Y1 - 2007/8/6
N2 - The reaction between 1,2-bis[3-(3,5-dimethyl-1-pyrazolyl)-2-thiapropyl]benzene (bddf) and [MCl2(CH3CN)2] (M = Pd(II), Pt(II)) in a 1:1 M/L ratio in CH2Cl2 or acetonitrile solution, respectively, gave the complexes trans-[MCl2(bddf)] (M = Pd(II) (1), Pt(II) (4)), and in a 2:1 M/L ratio led to [M2Cl4(bddf)] (M = Pd(II) (2), Pt(II) (5)). Treatment of 1 and 4 with AgBF4 and NaBPh4, respectively, gave the compounds [Pd(bddf)](BF4)2 (3) and [Pt(bddf)](BPh4)2 (6). When complexes 3 and 6 were heated under reflux in a solution of Et4NBr in CH2Cl2/CH3OH (1:1) for 24 h, analogous complexes to 1 and 4 with bromides instead of chlorides bonded to the metallic centre were obtained. These complexes were characterised by elemental analyses, conductivity measurements, infrared, 1H, 1H{195Pt}, 13C{1H}, 195Pt{1H} NMR, HSQC and NOESY spectroscopies. The X-ray crystal structure of the complex [Pd(bddf)](BF4)2 · H2O has been determined. The metal atom is tetracoordinated by the two azine nitrogen atoms of the pyrazole rings and two thioether groups. © 2007 Elsevier Ltd. All rights reserved.
AB - The reaction between 1,2-bis[3-(3,5-dimethyl-1-pyrazolyl)-2-thiapropyl]benzene (bddf) and [MCl2(CH3CN)2] (M = Pd(II), Pt(II)) in a 1:1 M/L ratio in CH2Cl2 or acetonitrile solution, respectively, gave the complexes trans-[MCl2(bddf)] (M = Pd(II) (1), Pt(II) (4)), and in a 2:1 M/L ratio led to [M2Cl4(bddf)] (M = Pd(II) (2), Pt(II) (5)). Treatment of 1 and 4 with AgBF4 and NaBPh4, respectively, gave the compounds [Pd(bddf)](BF4)2 (3) and [Pt(bddf)](BPh4)2 (6). When complexes 3 and 6 were heated under reflux in a solution of Et4NBr in CH2Cl2/CH3OH (1:1) for 24 h, analogous complexes to 1 and 4 with bromides instead of chlorides bonded to the metallic centre were obtained. These complexes were characterised by elemental analyses, conductivity measurements, infrared, 1H, 1H{195Pt}, 13C{1H}, 195Pt{1H} NMR, HSQC and NOESY spectroscopies. The X-ray crystal structure of the complex [Pd(bddf)](BF4)2 · H2O has been determined. The metal atom is tetracoordinated by the two azine nitrogen atoms of the pyrazole rings and two thioether groups. © 2007 Elsevier Ltd. All rights reserved.
KW - Crystal structures
KW - Hybrid ligands
KW - N ligands
KW - Palladium(II)
KW - Platinum(II)
KW - Pyrazole complexes
KW - S ligands
U2 - 10.1016/j.poly.2007.01.051
DO - 10.1016/j.poly.2007.01.051
M3 - Article
SN - 0277-5387
VL - 26
SP - 2921
EP - 2928
JO - Polyhedron
JF - Polyhedron
IS - 13
ER -