[NiCl2(C14H12N2)(H2O)] complex has been synthesized from nickel chloride hexahydrate (NiCl2·6H2O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as N,N-bidentate ligand. The synthesized complex was characterized by elemental analysis, infrared (IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy and differential thermal/thermogravimetric analysis (TG/DTA). The complex was further confirmed by single crystal X-ray diffraction (XRD) as triclinic with space group P-1. The desired complex, subjected to thermal decomposition at low temperature of 400 ºC in an open atmosphere, revealed a novel and facile synthesis of pure NiO nanoparticles with uniform spherical particle; the structure of the NiO nanoparticles product was elucidated on the basis of Fourier transform infrared (FT-IR), UV-vis spectroscopy, TG/DTA, XRD, scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDXS) and transmission electron microscopy (TEM).
Treatment of the dimers [RuX2(eta(6)-cymene)]2 with PF3 in hot heptane produces the compounds [RuX2(eta(6)-cymene)(PF3)] (X = Cl, Br, I) in good yield. Difluoro(dimethylamino)phosphine and tris(dimethylamino)phosphine react similarly to produce the compounds [RuX2(eta(6)-cymene)(PF2{NMe2})] and [RuX2(eta(6)-cymene)(P{NMe2}3)]. Reaction of the dimers [RuX2(eta(6)-cymene)]2 with PCl3 and PBr3 proceeded with the production of mononuclear products which had undergone halogen exchange at ruthenium in some cases. (1)H, (13)C, (31)P, and (19)F NMR spectra have been obtained where appropriate together with ((1)H-(1)H) correlation spectroscopy (COSY) and ((13)C-(1)H)-HETCORR spectra of selected compounds. The variation of (1)J((31)P-(19)F) with the nature of the auxiliary ligand (X) in the PF3 and PF2(NMe2) complexes has been examined both experimentally and computationally using a natural localized molecular orbital-natural bond order approach. The single crystal X-ray structure of [RuBr2(eta(6)-cymene)(PF3)] has been determined at 223 K and those of [RuBr2(eta(6)-cymene)(PF2{NMe2})] and [RuI2(eta(6)-cymene)(P{NMe2}3)] at 294 K.
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