Journal of Organometallic Chemistry p. 1172 - 1179 (2004)
Update date:2022-08-04
Topics:
Bumbu, Oana
Silvestru, Cristian
Concepción Gimeno
Laguna, Antonio
[2-(Me2NCH2)C6H4]HgCl (1) was prepared by reacting HgCl2 with [2-(Me2 NCH2)C6H4]Li in diethyl ether. The reactions of 1 with the sodium or ammonium salt of the appropriate thiophosphinato ligand, in 1:1 molar ratio, afford the isolation of [2-(Me2NCH2)C6H4]Hg[S(S) PR2] [R=Me (2), Et (3), Ph (4)], [2-(Me2 NCH2)C6H4]Hg[S(O)PPh2] (5) and [2-(Me2NCH2)C6H4] Hg[S(S)P(OiPr)2] (6). The compounds were investigated by IR and multinuclear NMR (1H, 13C and 31P) spectroscopy. The molecular structures of 1 and 4 were determined by single-crystal X-ray diffraction. Due to the strong intramolecular coordination of the N atom of the pendant CH2NMe2 arm [Hg((1)-N(1) 2.764(6) and 2.725(4) ? in 1 and 4, respectively] both compounds exhibit a T-shaped (C,N)HgX core in the molecular unit, with almost linear arrangement of the covalent bonds [C(1)-Hg(1)-Cl(1) 176.93(18)° in 1, and C(1)-Hg(1)-S(1) 169.54(16)° in 4]. The crystals of 1 contain discrete monomeric molecules, while the crystals of 4 contain dimer associations built through asymmetric bridging dithiophosphinato ligands [Hg(1)-S(1) 2.3911(16) ?, Hg(1)·S(2a) 3.102(2) ?], thus resulting in an overall pseudo-trigonal bipyramidal (or seesaw) (C, N)HgS2 core, with the nitrogen atom and the weekly bonded sulfur atom in equatorial positions [N(1)-Hg(1)·S(2a) 82.01(10)°].
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