Synthesis and Crystal Structure of Bis[O,O'-bis(4-tert-butylphenyl)dithiophosphate]nickel(Ⅱ)

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A new O,O’-bis(4-tert-butylphenyl)dithiophosphate complex Ni[SSP(OC6H4But- p)2]2 (1) was synthesized and characterized by elemental analysis, IR, 1H NMR, thermogravimetric analysis (TGA) and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 12.8440(3), b = 6.18686(12), c=26.3018(5) , β=92.6135(18)°, V = 2087.87(7) 3, Z = 2, Dc = 1.345 g/cm3, μ = 0.780 mm-1, the final R = 0.0316 and wR = 0.0748 (Ⅰ >2σ(Ⅰ)). A total of 4269 unique reflections were collected, of which 3621 with Ⅰ > 2σ(Ⅰ) were observed. The NiII atom lies on an inversion center and is chelated by two (p-ButC6H4O)2PSS-ligands in a [NiS4] square-planar geometry with Ni-S bonds of 2.2408(5) and 2.2444(5) , respectively. A stepwise 1D chain structure is constructed via intermolecular S…S and C-H…S interactions. According to our knowledge this is the first case that intermolecular S…S interaction is observed in mononuclear transition metal complex of O,O’-dialkyldithiophosphates. A new O, bis (4-tert-butylphenyl) dithiophosphate complex Ni [SSP (OC6H4But-p) 2] 2 synthesized by elemental analysis, IR, 1H NMR, thermogravimetric analysis (TGA) The crystal belongs to the monoclinic system, space group P21 / c with a = 12.8440 (3), b = 6.18686 (12) and c = 26.3018 (5) °, V = 2087.87 (7) 3, Z = 2, Dc = 1.345 g / cm3, μ = 0.780 mm-1, the final R = 0.0316 and wR = 0.0748 (I> 2σ (I) 4269 unique reflections were collected, of which 3621 with I> 2σ (Ⅰ) were observed. The NiII atom lies on an inversion center and is chelated by two (p-ButC6H4O) 2PSS-ligands in a [NiS4] Ni-S bonds of 2.2408 (5) and 2.2444 (5) , respectively. A stepwise 1D chain structure is constructed via intermolecular S ... S and CH ... S interactions. According to our knowledge this is the first case that intermolecular S ... S interaction is observed in mononuclear transition metal compl ex of O, O’-dialkyldithiophosphates.
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