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Abstract
The reaction of 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (Lawesson's Reagent) with two different Grignard reagents gave the corresponding dithiophos-phinic acids (DTPA), CH3OC6H4-(R)P(S)SH; [R = iso-butyl (HL1) and sec-butyl (HL2)]. HL1 and HL2 were treated with dry ammonia to convert them to the ammonium salts, NH4L1 and NH4L2. Ni(II) and Co(II) complexes of L1 and L2 – [Ni(L1)2], [Ni(L2)2]; [Co(L1)2]2 and [Co(L2)2]2—were obtained by the reaction of NH4L1 and NH4L2 with NiCl2.6H2O and CoCl2.6H2O, respectively, in ethanol. Square-planar nickel complexes [Ni(L1)2] and [Ni(L2)2] were further reacted with pyridine (Py) to obtain the octahedral complexes, [Ni(Py)2(L1)2] and [Ni(Py)2(L2)2]. The compounds were characterized by elemental analysis, FTIR, APCI/ESI-MS and 1H, 13C, and 31P NMR spectroscopies. The novel nickel(II) complex [Ni(L2)2] was characterized by X-ray crystallography.
Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental resource: Figures S1-S5.
GRAPHICAL ABSTRACT
Acknowledgments
The authors gratefully acknowledge the financial assistance of the Technical Research Council of Turkey (grant number TBAG 110T016, TUBITAK) and the Ankara University Research and Development Fund (grant number DPT-2002-K-120130-5). We thank also Anadolu University and Medicinal Plants and Medicine Research Center of Anadolu University, Eskişehir, Turkey, for allowing us to use the X-ray facility.