New methoxo-, hydroxo- and pyrazolate-bridged platinum(II) complexes. Crystal structure of [NBu4]2[{Pt(C6F5)2}2(µ-OH)(µ-dmpz)](dmpz = 3,5-dimethylpyrazolate)

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Abstract
The hydroxo complex [{Pt(C6F5)2(µ-OH)}2]2– reacts with azoles (1 : 1 molar ratio) in benzene to give the double bridged complexes [{Pt(C6F5)2}2(µ-OH)(µ-L–L)]2–[L–L = pyrazolate (pz)1, 3,5-dimethyl-pyrazolate (dmpz)2, 3-methylpyrazolate (mpz)3 or indazolate(indz)4]. When the same reaction is carried out in methanol with the reactants in 1 : 2 molar ratio the corresponding di-µ-azolate derivatives [{Pt(C6F5)2(µ-L–L)}2]2–[L–L = pz 5, dmpz 6, mpz 7 or indz 8] are obtained. On treatment of [{Pt(C6F5)2(µ-OH)}2]2– with methanol the di-µ-methoxo complex [{Pt(C6F5)2(µ-OMe)}2]2–9 was obtained. The di-µ-azolate complexes 5–8 can be alternatively prepared by treatment of 9 with the respective azoles (1 : 2 molar ratio) in methanol. Reaction of complex 1 with methanol leads to the formation of [{Pt(C6F5)2}2(µ-OMe)(µ-pz)]2–10. All the complexes have been isolated as the [NBu4]+ salts. Spectroscopic (IR, 1H and 19F NMR) data have been used for structural assignments, and an X-ray structure determination carried out for [NBu4]2[{Pt(C6F5)2}2(µ-OH)(µ-dmpz)] has established the binuclear nature of the anion. The structure was solved and refined to R= 0.057 and R′= 0.089 based on 10 057 observed reflections. The Pt atoms are four-co-ordinated, Pt(1)–O 2.113(7), Pt(1)–N(1) 2.04(1), Pt(1)–C(10) 2.02(1), Pt(1)–C(20) 1.96(2), Pt(2)–O 2.077(9), Pt(2)–N(2) 2.075(9), Pt(2)–C(30) 1.97(2), Pt(2)–C(40) 2.00(1)Å, and show deviations from a square-planar arrangement towards a tetrahedral disposition.

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