名称:
Synthesis, structural characterisation and thermal decomposition of [{Pt(dppf)(2-SPy)}{BF4}] (dppf=1,1′-bisdiphenylphosfinoferrocene and 2-SPy=2-mercaptopyridine) – a source for a Fe–Pt containing alloy
摘要:
The reaction of 2-PySK with [Pt(dppf)Cl-2] [dppf = 1,1'-bis(diphenylphosfinofeffocene) and 2-PyS = 2-mercaptopyridine] produced Pt(dppf)(2-SPY)(2) (1) and its subsequent reaction with SnBu2(BF4)(2) or SnBu3(BF4) yielded [{Pt(dppf)(2-SPy)}{BF4}] (2). Compounds 1 and 2 were fully characterised by multinuclear NMR [H-1, C-13{H-1}, P-31{H-1} and Pt-195{H-1}] and Fe-57 Mossbauer spectroscopies. In addition the structure of 2 was determined by X-ray crystallographic studies, which can be summarised as follows: monoclinic P2(1)/c, a = 9.9291(9) Angstrom, b = 22.270(4) Angstrom, c = 16.919(2) Angstrom, y = 103.6(9)degrees, V = 3636.2(8) Angstrom(3) and Z = 4. Finally, a thermal decomposition study was carried out with 2 in three different atmosphere: oxygen, nitrogen or hydrogen. The residues were characterised by X-ray powder diffraction (XRD), X-ray electron probe microanalysis (EPMA), scanning electron microscopy (SEM) and Fe-57 Mossbauer spectroscopy. The results have shown the formation of a disordered Pt1-xFex based alloy when the pyrolysis process was performed in H-2, simultaneously with small amount of Fe(II) and Fe(III) phosphides. Furthermore, in oxygen and nitrogen the thermal decomposition of 2 produced metallic agglomerate's of Pt dispersed in a combination of Fe(II) and Fe(III) phosphates in O-2, and an intricate mixture of sulphides and phosphides in N-2. (C) 2003 Elsevier Ltd. All rights reserved.