trans-Di-μ-chlorido-bis­{chlorido[tris­(3,5-dimethyl­phen­yl)phosphane-κP]palla­dium(II)} dichloro­methane monosolvate

Davis, W.L.; Muller, A.

doi:10.1107/S1600536812048556

Volume 68
Part 12
Pages m1563-m1564
December 2012

Received 24 November 2012
Accepted 26 November 2012
Online 30 November 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.005 Å
R = 0.040
wR = 0.098
Data-to-parameter ratio = 23.3
Details

trans-Di--chlorido-bis{chlorido[tris(3,5-dimethylphenyl)phosphane-P]palladium(II)} dichloromethane monosolvate

Wade L. Davis ^a and Alfred Muller ^a ^*

^aResearch Centre for Synthesis and Catalysis, Department of Chemistry, University of Johannesburg (APK Campus), PO Box 524, Auckland Park, Johannesburg, 2006, South Africa
Correspondence e-mail: mullera@uj.ac.za

In the dimeric title compound, [Pd₂Cl₄{P(C₈H₉)₃}₂]·CH₂Cl₂, the metal complex molecule is situated about an inversion centre and is accompanied by a dichloromethane solvent molecule situated on a twofold rotation axis. The Pd^II atom has a slightly distorted square-planar coordination sphere. The effective cone angle for the tris(3,5-dimethylphenyl)phosphane ligand was calculated to be 169°. In the crystal, the metal complex and solvent molecules are linked via C-HCl interactions, generating chains along [10-2]. There are also C-H [pi] and weak [pi] - [pi] interactions present [centroid-centroid distance = 3.990 (2) Å, plane-plane distance = 3.6352 (15) Å and ring slippage = 1.644 Å], forming of a three-dimensional structure.

Related literature

For background on catalysis of palladium compounds, see: Bedford et al. (2004). For the synthesis of the starting materials, see: Drew & Doyle (1990). For a description of the Cambridge Structural Database, see: Allen (2002). For background on cone angles, see: Tolman (1977); Otto (2001).

Experimental

Crystal data

[Pd₂Cl₄(C₂₄H₂₇P)₂]·CH₂Cl₂
M_r = 1132.38
Monoclinic, P 2/c
a = 14.747 (2) Å
b = 9.1038 (13) Å
c = 21.376 (3) Å
= 117.576 (8)°
V = 2543.8 (6) Å³
Z = 2
Mo K radiation
= 1.12 mm^-1
T = 100 K
0.19 × 0.16 × 0.13 mm

Data collection

Bruker APEX DUO 4K-CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008) T_min = 0.816, T_max = 0.868
30952 measured reflections
6349 independent reflections
4776 reflections with I > 2(I)
R_int = 0.071

Refinement

R[F² > 2(F²)] = 0.040
wR(F²) = 0.098
S = 1.03
6349 reflections
273 parameters
H-atom parameters constrained
_max = 0.90 e Å^-3
_min = -1.12 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

Cg1 and Cg2 are the centroids of rings C17-C19/C21/C22/C24 and C9-C11/C13/C14/C16, respectively.

D-HA	D-H	HA	DA	D-HA
C25-H25ACl2	0.99	2.82	3.733 (4)	154
C21-H21Cl1ⁱ	0.95	2.85	3.693 (4)	148
C5-H5Cg1ⁱⁱ	0.95	2.95	3.847 (5)	159
C15-H15ACg2ⁱⁱⁱ	0.99	2.79	3.620 (5)	143
Symmetry codes: (i) $[-x+1, y, -z+{\script{1\over 2}}]$ ; (ii) -x+2, -y+1, -z+1; (iii) -x+1, -y+2, -z+1.

Data collection: APEX2 (Bruker, 2011); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT and XPREP (Bruker, 2008); 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, 2005); software used to prepare material for publication: publCIF (Westrip, 2010) and WinGX (Farrugia, 2012).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2534 ).

Acknowledgements

Financial assistance from the Research Fund of the University of Johannesburg is gratefully acknowledged. Mrs Z. Phasha is thanked for the data collection.

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.
Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.
Bedford, R. B., Cazin, C. S. J. & Holder, D. (2004). Coord. Chem. Rev. 248, 2283-2321.
Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2008). SADABS, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Drew, D. & Doyle, J. R. (1990). Inorg. Synth. 28, 346-349.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
Otto, S. (2001). Acta Cryst. C57, 793-795.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Tolman, C. A. (1977). Chem. Rev. 77, 313-348.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.

metal-organic compounds