Bis[N,N-bis(diphenylphosphanyl)pentylamine-κ2 P,P′]platinum(II) bis(hexafluoridophosphate) dichloromethane disolvate

The PtII atom in the title compound, [Pt(C29H31NP2)2](PF6)2·2CH2Cl2, is coordinated by four P atoms from two bis(diphenylphosphanyl)pentylamine ligands with an average Pt—P distance of 2.300 (1) Å. The coordination around the PtII atom shows a highly distorted square-planar geometry, as evidenced by the P—Pt—P bite angles of 70.45 (3) and 70.64 (3)°. The asymmetric unit contains two hexafluoridophosphate ions, the metal complex and two dichloromethane solvent molecules. One of the chloride atoms of one of the dichloromethane molecules is disordered over two sites in a 0.515 (3):0.485 (3) ratio. C—H⋯F hydrogen bonds stabilize the crystal packing.

The Pt II atom in the title compound, [Pt(C 29 H 31 NP 2 ) 2 ](PF 6 ) 2 Á-2CH 2 Cl 2 , is coordinated by four P atoms from two bis(diphenylphosphanyl)pentylamine ligands with an average Pt-P distance of 2.300 (1) Å . The coordination around the Pt II atom shows a highly distorted square-planar geometry, as evidenced by the P-Pt-P bite angles of 70.45 (3) and 70.64 (3) . The asymmetric unit contains two hexafluoridophosphate ions, the metal complex and two dichloromethane solvent molecules. One of the chloride atoms of one of the dichloromethane molecules is disordered over two sites in a 0.515 (3):0.485 (3) ratio. C-HÁ Á ÁF hydrogen bonds stabilize the crystal packing.

Experimental
Crystal data [Pt(C 29

Comment
The synthesis of diphenylphosphanyl ligands and metal complexes thereof, forms part of ongoing research in the field of homogeneous catalysis (Steyn et al., 1992(Steyn et al., , 1997Otto et al., 1998;Roodt & Steyn, 2000;Brink et al., 2010;Viljoen et al., 2008Viljoen et al., , 2009aViljoen et al., ,b, 2010Steyn et al., 2008). Colourless crystals of the title compound crystallize with two hexafluoridophosphate anions and two dichloromethane solvent molecules, of which one displays a 51% possitional disorder on one chloride atom. In the title compound, all bond distances and angles are considered to be normal and fall within the range reported for similar complexes (Farrar et al., 1995;Dyson et al., 2004;Cloete et al., 2010). The square-planar geometry around the Pt II metal centre is highly distorted with P1-Pt-P2 and P3-Pt-P4 bite angles of 70.45 (3) and 70.64 (3) °, respectively. The distorted tetrahedral angles of the P atoms, which range between 92.81 (9) and 122.28 (11) ° further illustrate the strain in the complex. The N atoms also deviate from the ideal tetrahedral configuration with P1-N1-P2 and P3-N2-P4 angles being 103.40 (13) and 103.15 (13) °, respectively. The distance between the N1 atom and the plane created by C1, P1 and P2 is -0.021 (2) ° whereas the distance of N2 and the plane created by C6, P3 and P4 shows a slightly bigger deviation of -0.122 (2) °. This shows that the N atom adopts an almost planar geometry with the two P atoms and the C atom attached to it in each case to accomodate the steric bulk of the phenyl groups and the alkyl group of the ligand. The intermolecular hydrogen bonds lead to a three-dimensional polymetric network obtained through C-H···F interactions.

Experimental
[Pt(cod)Cl 2 ] (20 mg, 0.0535 mmol) (cod = 1,5-cyclooctadiene) dissolved in the minimum amount of dichloromethane was added in a rapid dropwise manner to a solution of bis(diphenylphosphanyl)pentylamine (51.9 mg, 0.114 mmol) and NaPF 6 (20 mg, 0.119 mmol) dissolved in the minimum volume of dichloromethane-methanol (1:1). After stirring for 20 min, the solvent was removed completely under reduced pressure. Dichloromethane was added until no further dissolution of solid was evident. The resulting heterogeneous mixture was filtered to remove the insoluble NaCl by-product. The colourless solid product was precipitated upon addition of methanol followed by a reduction in solvent volume under reduced pressure.

Refinement
The methyl, methylene and aromatic H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with C-H = 0.95, 0.99 and 0.98Å and Uĩso~(H) = 1.5U~eq~(C) and 1.2U~eq~(C), respectively.The methyl groups were generated to fit the difference electron density and the groups were then refined as rigid rotors. The highest peak is located 0.06Å from C1 and the deepest hole is situated 0.06Å from C02B. Fig. 1. Molecular structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. Hydrogen atoms, solvent molecules and hexafluoridophosphate ions have been omitted for clarity and are displayed in Figure 2.

Special details
Experimental. The intensity data was collected on a Bruker X8 ApexII 4 K Kappa CCD diffractometer using an exposure time of 30 s/frame. A total of 1757 frames were collected with a frame width of 0.5° covering up to θ = 28.32° with 99.1% completeness accomplished.
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The 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 > 2σ(F 2 ) is used only for calculating Rfactors(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.