trans-Bis(4-methoxythiophenolato-κS)bis(trimethylphosphine-κP)nickel(II)

The title compound, [Ni(C7H7OS)2(C3H9P)2], was obtained as a product of the reaction of [NiMe2(PMe3)3] with two molar equivalents of 4-methoxythiophenol in diethyl ether. The compound is stable in the air for several hours, but rapidly decomposes at room temperature in solution. The Ni atom displays a square-planar coordination with two P-donor atoms lying in trans positions. The benzene rings of the thiophenolate ligands are almost perpendicular to the square coordination plane, making dihedral angles of 80.43 (4) and 72.60 (4)°.

The title compound, [Ni(C 7 H 7 OS) 2 (C 3 H 9 P) 2 ], was obtained as a product of the reaction of [NiMe 2 (PMe 3 ) 3 ] with two molar equivalents of 4-methoxythiophenol in diethyl ether. The compound is stable in the air for several hours, but rapidly decomposes at room temperature in solution. The Ni atom displays a square-planar coordination with two P-donor atoms lying in trans positions. The benzene rings of the thiophenolate ligands are almost perpendicular to the square coordination plane, making dihedral angles of 80.43 (4) and 72.60 (4) .

S1. Comment
In the title molecule ( Fig.1) the nickel atom is coordinated in a square-planar geometry by two P atoms of trimethylphosphine groups and two S atoms of thiophenol groups. The phenyl rings of the thiophenlato ligands are almost perpendicular to the square coordination plane (angles 80.43 (4)° and 72.60 (4)°). Similar crystal structures have been reported in the literature, e.g. Bis(2-tert-butyl-4-methylphenolato)bis(trimethylphosphane)nickel and Bis(2-tert-butyl-6methylphenolato)bis(trimethylphosphane)nickel (Klein et al.(1998)). The bond lengths and angles of these compounds are similar to those in the title compound.

S2. Experimental
Dimethyltris(trimethylphosphine)nickel was prepared according to the literature (Klein & Karsch (1972)). Other chemicals were used by purchased. To the solution of NiMe 2 (PMe 3 ) 3 (1.0 g, 3.15 mmol) in 50 ml of diethyl ether was added 4-methoxythiophenol (0.884 g, 6.30 mmol) at -80 °C, a dark red suspension formed rapidly. After stirring at room temperature for 16 h the reaction solution was filtrated, then the red solid residue was extracted with THF (50 ml).

Figure 1
The molecular structure of (I), with a 30% probability displacement ellipsoids for non-H atoms.

Crystal data
[Ni(C 7 H 7 OS) 2 (C 3 H 9 P) 2 ] M r = 489.23 Monoclinic, P2 1 /c Hall symbol: -P 2ybc a = 14.022 (3)  where P = (F o 2 + 2F c 2 )/3 (Δ/σ) max = 0.001 Δρ max = 0.34 e Å −3 Δρ min = −0.47 e Å −3 Special details Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > σ(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.