[1,2-Bis(diphenylphosphino)ethane-κ2 P,P′](2-carboxylatothiophenolato-κ2 O,S)nickel(II) methanol solvate

In the title complex, [Ni(C7H4O2S)(C26H24P2)]·CH3OH, the nickel(II) centre adopts an approximately square-planar geometry, with the Ni atom coordinating to the S and O atoms of the bidentate thiosalicylate ligand and the two P atoms of the chelating Ph2PCH2CH2PPh2 ligand. There is hydrogen bonding between the methanol solvent molecule and the carbonyl O atom of the thiosalicylate ligand.

In the title complex, [Ni(C 7 H 4 O 2 S)(C 26 H 24 P 2 )]ÁCH 3 OH, the nickel(II) centre adopts an approximately square-planar geometry, with the Ni atom coordinating to the S and O atoms of the bidentate thiosalicylate ligand and the two P atoms of the chelating Ph 2 PCH 2 CH 2 PPh 2 ligand. There is hydrogen bonding between the methanol solvent molecule and the carbonyl O atom of the thiosalicylate ligand.

Related literature
For previous preparations and structures of the non-solvated complex, see: Kang et al. (1998);McCaffrey et al. (1997).

Experimental
Crystal data [Ni(C 7 Table 1 Selected geometric parameters (Å , ).  Hydrogen-bond geometry (Å , ). complex as a methanol solvate when NiCl 2 (dppe) was reacted with thiosalicylic acid in the presence of NaOH as a base.
As shown in Fig. 1, the coordination geometry around the nickel center is approximately square planar. The sum of the bond angles around the Ni atom is 359.92°, with the trans P-Ni-S and P-Ni-O angles being 172.70 and 178.81°, respectively, Table 1, while in related structures the corresponding values were found to be 361. 45, 170.99 and170.73° (McCaffrey et al., 1997), and358.4, 166.0, 173.0°, (Kang et al., 1998) respectively. These indicate that in the present structure the P 2 OS unit is slightly more planar. As expected, the Ni1-P2 bond length (opposite to S, 2.2114 (10) Å) is found to be longer than that for Ni1-P1 (opposite to O, 2.1378 (11) Å), due to the different trans influence of the S and O atoms. Strong O3-H3···O2 i [i = x, -y + 1/2, z -1/2] hydrogen bonding (2.697 Å) is observed between the methanol solvate molecule and the carbonyl O atom of the thiosalicylato group, Table 2.

S3. Refinement
All H atoms were positioned geometrically and refined using a riding model with d(C-H) = 0.93 Å, U iso = 1.2U eq (C) for aromatic, 0.97 Å, U iso = 1.2U eq (C) for CH 2 , 0.96 Å, U iso = 1.5U eq (C) for CH 3 atoms and 0.82 Å, U iso = 1.5U eq (O) for the OH groups.  The molecular structure, with atom labels and 25% probability displacement ellipsoids for non-H atoms.
Special details 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 > 2sigma(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.