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Volume 68 
Part 12 
Pages m1508-m1509  
December 2012  

Received 13 November 2012
Accepted 15 November 2012
Online 24 November 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.003 Å
Disorder in main residue
R = 0.032
wR = 0.077
Data-to-parameter ratio = 16.5
Details
Open access

trans-Dichloridobis{tris[4-(trifluoromethyl)phenyl]phosphane-[kappa]P}palladium(II) dichloromethane monosolvate

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

The title compound, [PdCl2(C21H12F9P)2]·CH2Cl2, crystallizes with two independent complex molecules (each having the PdII atom situated on an inversion centre) and a dichloromethane molecule in the asymmetric unit. The independent PdII atoms are in perfectly linear orientations of the ligands in mutually trans positions, but distortions of the Cl-Pd-P angles ranging from 86.151 (19) to 93.849 (19)° are evident. The effective cone angles for the tris[4-(trifluoromethyl)phenyl]phosphane ligand were calculated to be 159 and 161°. In the crystal, weak C-H...Cl/F interactions create a three-dimensional supramolecular network. Loose packing at two of the -CF3 groups resulted in large thermal vibrations which were treated as two-component disorders [occupancy ratios 0.50:0.50 and 0.628 (15):0.372 (15)].

Related literature

For background to catalysis of palladium compounds, see: Bedford et al. (2004[Bedford, R. B., Cazin, C. S. J. & Holder, D. (2004). Coord. Chem. Rev. 248, 2283-2321.]). For a description of the Cambridge Structural Database, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]). For background to cone angles, see: Tolman (1977[Tolman, C. A. (1977). Chem. Rev. 77, 313-348.]); Otto (2001[Otto, S. (2001). Acta Cryst. C57, 793-795.]). For details of the conformational fit between molecules using Mercury, see: Macrae et al. (2006[Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457.]); Weng et al. (2008a[Weng, Z. F., Motherwell, W. D. S., Allen, F. H. & Cole, J. M. (2008a). Acta Cryst. B64, 348-362.],b[Weng, Z. F., Motherwell, W. D. S. & Cole, J. M. (2008b). J. Appl. Cryst. 41, 955-957.]).

[Scheme 1]

Experimental

Crystal data
  • [PdCl2(C21H12F9P)2]·CH2Cl2

  • Mr = 1194.78

  • Triclinic, [P \overline 1]

  • a = 12.1491 (10) Å

  • b = 14.0203 (13) Å

  • c = 14.4334 (13) Å

  • [alpha] = 72.764 (2)°

  • [beta] = 78.362 (2)°

  • [gamma] = 75.545 (2)°

  • V = 2252.0 (3) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.83 mm-1

  • T = 100 K

  • 0.34 × 0.31 × 0.25 mm

Data collection
  • Bruker APEX DUO 4K CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). SADABS, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.766, Tmax = 0.820

  • 48517 measured reflections

  • 11209 independent reflections

  • 9475 reflections with I > 2[sigma](I)

  • Rint = 0.03

Refinement
  • R[F2 > 2[sigma](F2)] = 0.032

  • wR(F2) = 0.077

  • S = 1.02

  • 11209 reflections

  • 680 parameters

  • 116 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 1.14 e Å-3

  • [Delta][rho]min = -0.85 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C12-H12...Cl3 0.95 2.78 3.468 (2) 130
C7-H7B...Cl4 0.99 2.54 3.510 (4) 165
C65-H65...F6i 0.95 2.55 3.457 (3) 160
C7-H7A...Cl3ii 0.99 2.57 3.550 (5) 169
C15-H15...F17Aiii 0.95 2.52 3.341 (6) 144
C33-H33...F10B 0.95 2.53 3.435 (4) 159
Symmetry codes: (i) -x, -y+1, -z; (ii) -x, -y, -z+1; (iii) x-1, y, z-1.

Data collection: APEX2 (Bruker, 2011[Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). SADABS, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT and XPREP (Bruker, 2008[Bruker (2008). SADABS, SAINT and XPREP. Bruker AXS Inc., Madison, Wisconsin, USA.]); program(s) used to solve structure: SIR97 (Altomare et al., 1999[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.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg & Putz, 2005[Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]) and WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: ZQ2189 ).


Acknowledgements

Financial assistance from the Research Fund of the University of Johannesburg is gratefully acknowledged.

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.  [ISI] [CrossRef] [details]
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.  [ISI] [CrossRef] [ChemPort] [details]
Bedford, R. B., Cazin, C. S. J. & Holder, D. (2004). Coord. Chem. Rev. 248, 2283-2321.  [ISI] [CrossRef] [ChemPort]
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.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457.  [ISI] [CrossRef] [ChemPort] [details]
Otto, S. (2001). Acta Cryst. C57, 793-795.  [CSD] [CrossRef] [ChemPort] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Tolman, C. A. (1977). Chem. Rev. 77, 313-348.  [CrossRef] [ChemPort] [ISI]
Weng, Z. F., Motherwell, W. D. S., Allen, F. H. & Cole, J. M. (2008a). Acta Cryst. B64, 348-362.  [ISI] [CrossRef] [details]
Weng, Z. F., Motherwell, W. D. S. & Cole, J. M. (2008b). J. Appl. Cryst. 41, 955-957.  [ISI] [CrossRef] [ChemPort] [details]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]


Acta Cryst (2012). E68, m1508-m1509   [ doi:10.1107/S1600536812046971 ]

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