[N,N-Bis(diphenyl­phosphino)propyl­amine-κ2 P,P′]dichloridoplatinum(II)

Nicoline Cloete; Hendrik G Visser; Andreas Roodt

doi:10.1107/S160053680905301X

. 2009 Dec 12;66(Pt 1):m51–m52. doi: 10.1107/S160053680905301X

[N,N-Bis(diphenylphosphino)propylamine-κ² P,P′]dichloridoplatinum(II)

Nicoline Cloete ^a,^*,^‡, Hendrik G Visser ^a, Andreas Roodt ^a

PMCID: PMC2980280 PMID: 21579949

Abstract

The Pt(II) atom in the title compound, [PtCl₂(C₂₇H₂₇NP₂)], has a highly distorted square-planar geometry, as evidenced by the P—Pt—P bite angle [72.4 (1)°]. The strain in the complex is further illustrated by the distorted tetrahedral angles of the P atoms, which range between 93.5 (1) and 122.2 (1)°. It is of interest to note that the N atom has to adopt an almost planar geometry with the two P atoms and the C atom attached to it [it is displaced by 0.093 (2) Å from the CP₂ plane] in order to accommodate the steric bulk of the phenyl groups and the alkyl group of the ligand coordinated to the Pt^II centre. The molecules pack in horizontal rows across the bc plane. C—H⋯Cl hydrogen bonds stabilize the crystal packing.

Related literature

For related platinum(II) complexes, see: Browning et al. (1992 ▶); Calabrò et al. (2004 ▶); Fei et al. (2006 ▶).

Experimental

Crystal data

[PtCl₂(C₂₇H₂₇NP₂)]
M _r = 693.43
Monoclinic,
a = 10.6301 (4) Å
b = 18.8117 (7) Å
c = 12.7653 (5) Å
β = 97.326 (1)°
V = 2531.84 (17) Å³
Z = 4
Mo Kα radiation
μ = 5.90 mm⁻¹
T = 101 K
0.38 × 0.10 × 0.02 mm

Data collection

Bruker X8 APEXII Kappa CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T _min = 0.213, T _max = 0.891
50743 measured reflections
6276 independent reflections
5347 reflections with I > 2σ(I)
R _int = 0.052

Refinement

R[F ² > 2σ(F ²)] = 0.022
wR(F ²) = 0.053
S = 1.04
6276 reflections
298 parameters
H-atom parameters constrained
Δρ_max = 1.55 e Å⁻³
Δρ_min = −0.63 e Å⁻³

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 1999 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680905301X/hy2248sup1.cif

e-66-00m51-sup1.cif^{(24.1KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S160053680905301X/hy2248Isup2.hkl

e-66-00m51-Isup2.hkl^{(301KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

Pt—P1	2.1932 (7)
Pt—P2	2.2121 (7)
Pt—Cl1	2.3461 (7)
Pt—Cl2	2.3528 (7)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1A⋯Cl1ⁱ	0.99	2.64	3.512 (3)	147

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Symmetry code: (i) Inline graphic .

Acknowledgments

Financial assistance from the South African National Research Foundation (NRF), the Research Fund of the University of the Free State and SASOL is gratefully acknowledged. Dr M. J. Janse van Rensburg is gratefully acknowledged for the collection of the data. Part of this material is based on work supported by the South African National Research Foundation (GUN 2038915). Opinions, findings, conclusions or recommendations expressed in this material are those of the authors and do not necessarily reflect the views of the NRF.

supplementary crystallographic information

Comment

In the title compound (Fig. 1 and Table 1), all bond distances and angles are considered to be normal and fall within range reported for similar complexes (Browning et al., 1992; Fei et al., 2006; Calabrò et al., 2004). The square-planar geometry of the complex is highly distorted with a P1—Pt—P2 bite angle of 72.40 (3)° and a Cl1—Pt—Cl2 angle of 92.7 (1). The reported P1—Pt—P2 small bite angle forces the P1—N1—P2 angle to 100.1 (1)° which illustrates the distorted geometry from the ideal tetrahedral geometry of the N atom. The distance between the N1 atom and the plane created by C1, P1 and P2 is 0.093 (2) Å. The P atoms are also severely distorted from the expected tetrahedral configuration with Pt—P1—N1 and Pt—P2—N1 angles being 94.0 (1) and 93.5 (1)°, respectively. The molecules of the title compound pack horizontal rows in the unit cell across the bc plane (Fig. 2). Intermolecular hydrogen bond exists between C1—H1A and Cl1(1/2+x, 1/2-y, -1/2+z) (Table 2).

Experimental

Pt(cod)Cl₂ (50 mg, 0.13 mmol) (cod = 1,5-cyclooctadiene) was dissolved in dichloromethane (15 ml). Bis(diphenylphosphino)propylamine (57.1 mg, 0.13 mmol) was also dissolved in dichloromethane (10 ml) and was added dropwise to the Pt(cod)Cl₂ solution. The solution was stirred for 2 h at room temperature. The reaction mixture was layered with methanol (10 ml). Colourless single crystals suitable for X-ray crystallography was obtained after 1 d (yield 0.066 g, 73.4%).