Bis[N,N-bis­(diphenyl­phosphan­yl)pentyl­amine-κ2P,P′]platinum(II) bis­(hexa­fluoridophosphate) dichloro­methane disolvate

Engelbrecht, I.; Visser, H.G.; Roodt, A.

doi:10.1107/S1600536810025560

Volume 66
Part 8
Pages m922-m923
August 2010

Received 24 June 2010
Accepted 29 June 2010
Online 14 July 2010

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.005 Å
Disorder in solvent or counterion
R = 0.024
wR = 0.047
Data-to-parameter ratio = 18.5
Details

Bis[N,N-bis(diphenylphosphanyl)pentylamine-²P,P']platinum(II) bis(hexafluoridophosphate) dichloromethane disolvate

Ilana Engelbrecht,^a ^* Hendrik G. Visser ^a and Andreas Roodt ^a

^aDepartment of Chemistry, University of the Free State, PO Box 339, Bloemfontein 9300, South Africa
Correspondence e-mail: engelbrechti@ufs.ac.za

The Pt^II 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 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-HF hydrogen bonds stabilize the crystal packing.

Related literature

For related platinum(II) complexes, see: Farrar & Browning (1995); Dyson et al. (2004); Cloete et al. (2010). For related diphenylphosphanyl ligands, see: Keat et al. (1981); Cloete et al. (2008, 2009); Cotton et al. (1996); Fei et al. (2003). For applications of diphenylphosphanyl ligands and their metal complexes in homogeneous catalysis, see: Steyn et al. (1992, 1997); Otto et al. (1998); Roodt & Steyn (2000); Brink et al. (2010); Viljoen et al. (2008, 2009a,b, 2010); Steyn et al. (2008).

Experimental

Crystal data

[Pt(C₂₉H₃₁NP₂)₂](PF₆)₂·2CH₂Cl₂
M_r = 1565.85
Monoclinic, C c
a = 11.3876 (10) Å
b = 24.283 (3) Å
c = 23.102 (2) Å
= 97.669 (4)°
V = 6331.1 (11) Å³
Z = 4
Mo K radiation
= 2.61 mm^-1
T = 100 K
0.26 × 0.19 × 0.13 mm

Data collection

Bruker X8 APEXII 4K Kappa CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2004) T_min = 0.550, T_max = 0.728
47664 measured reflections
14210 independent reflections
13180 reflections with I > 2(I)
R_int = 0.03

Refinement

R[F² > 2(F²)] = 0.024
wR(F²) = 0.047
S = 0.89
14210 reflections
767 parameters
2 restraints
H-atom parameters constrained
_max = 1.08 e Å^-3
_min = -1.13 e Å^-3
Absolute structure: Flack (1983), 6561 Friedel pairs
Flack parameter: 0.014 (2)

Table 1
Selected geometric parameters (Å, °)

P1-Pt1	2.3063 (8)
P2-Pt1	2.2965 (8)
P3-Pt1	2.2994 (8)
P4-Pt1	2.2995 (8)

P2-N1-P1	103.40 (13)
P4-N2-P3	103.15 (13)
N1-P1-Pt1	92.81 (9)
C41-P2-Pt1	118.82 (11)
C51-P3-Pt1	122.28 (11)
N2-P4-Pt1	93.11 (9)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C25-H25F8	0.95	2.53	3.437 (4)	160
C55-H55F2	0.95	2.49	3.079 (4)	120
C65-H65F10	0.95	2.47	3.297 (4)	145
C83-H83F11	0.95	2.37	3.267 (4)	158
C01-H01BF2ⁱ	0.99	2.29	3.244 (5)	161
C01-H01BF6ⁱ	0.99	2.4	3.150 (5)	132
C5-H5CF11ⁱⁱ	0.98	2.51	3.196 (4)	127
C8-H8AF3ⁱⁱⁱ	0.99	2.54	3.450 (4)	153
C53-H53F7^iv	0.95	2.51	3.273 (4)	137
C63-H63F4^v	0.95	2.51	3.373 (4)	151
C73-H73F9^vi	0.95	2.53	3.426 (4)	156
Symmetry codes: (i) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (ii) x-1, y, z; (iii) x+1, y, z; (iv) $[x, -y+1, z+{\script{1\over 2}}]$ ; (v) $[x+{\script{1\over 2}}, y-{\script{1\over 2}}, z]$ ; (vi) $[x-{\script{1\over 2}}, y+{\script{1\over 2}}, z]$ .

Data collection: APEX2 (Bruker, 2010); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT5278 ).

Acknowledgements

Financial assistance from the Department of Science and Technology (DST) of South Africa, the South African National Research Foundation (NRF), as well as the DST-NRF centre of excellence (c*change) and the University of the Free State are gratefully acknowledged.

References

Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Brink, A., Visser, H. G., Steyl, G. & Roodt, A. (2010). Dalton Trans. pp. 5572-5578.
Bruker (2004). SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2010). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Cloete, N., Visser, H. G. & Roodt, A. (2010). Acta Cryst. E66, m51-m52.
Cloete, N., Visser, H. G., Roodt, A., Dixon, J. T. & Blann, K. (2008). Acta Cryst. E64, o480.
Cloete, N., Visser, H. G., Roodt, A. & Gabrielli, W. F. (2009). Acta Cryst. E65, o3081.
Cotton, F. A., Kuhn, F. E. & Yokochi, A. (1996). Inorg. Chim. Acta, 252, 251-256.
Dyson, P. J., Fei, Z. & Scopelliti, R. (2004). Eur. J. Inorg. Chem. pp. 530-537.
Farrar, D. G. & Browning, C. S. (1995). J. Chem. Soc. Dalton Trans. pp. 521-530.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Fei, Z., Scopeleti, R. & Dyson, P. J. (2003). Dalton Trans. pp. 2772-2779.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Keat, R., Manojlovic-Muir, L., Muir, K. W. & Rycroft, D. S. (1981). J. Chem. Soc. Dalton Trans. pp. 2192-2198.
Otto, S., Roodt, A., Swarts, J. C. & Erasmus, J. C. (1998). Polyhedron, 17, 2447-2453.
Roodt, A. & Steyn, G. J. J. (2000). Recent Research Developments in Inorganic Chemistry, Vol. 2, pp. 1-23. Trivandrum, India: Transworld Research Network.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Steyn, G. J. J., Roodt, A. & Leipoldt, J. G. (1992). Inorg. Chem. 31, 3477-3481.
Steyn, G. J. J., Roodt, A., Poletaeva, I. A. & Varshavsky, Y. S. (1997). J. Organomet. Chem. 536-537, 197-205.
Steyn, M., Roodt, A. & Steyl, G. (2008). Acta Cryst. E64, m827.
Viljoen, J. A., Muller, A. & Roodt, A. (2008). Acta Cryst. E64, m838-m839.
Viljoen, J. A., Visser, H. G. & Roodt, A. (2010). Acta Cryst. E66, m603-m604.
Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009a). Acta Cryst. E65, m1514-m1515.
Viljoen, J. A., Visser, H. G., Roodt, A. & Steyn, M. (2009b). Acta Cryst. E65, m1367-m1368.