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Volume 68 
Part 12 
Pages m1565-m1566  
December 2012  

Received 19 November 2012
Accepted 24 November 2012
Online 30 November 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.007 Å
R = 0.052
wR = 0.154
Data-to-parameter ratio = 19.5
Details
Open access

Di-[mu]-chlorido-bis({8-[bis(naphthalen-1-yl)phosphanyl]naphthalen-1-yl-[kappa]2C1,P}palladium(II)) dichloromethane disolvate

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, [Pd2{P(C10H7)2(C10H6)}2Cl2]·2CH2Cl2, shows cyclometalation of one naphthalen-1-yl substituent of each of the phosphane ligands to the Pd dimer in a trans orientation; the complete dimer is generated by a centre of inversion. Two dichloromethane solvent molecules create C-H...Cl interactions with the metal complex, generating supermolecular layers in the ab plane. Additional C-H...[pi] and [pi]-[pi] [centroid-centroid distances = 3.713 (3), 3.850 (4) and 3.926 (3) Å] interactions join these planes into a three-dimensional supermolecular network.

Related literature

For background to palladium compounds in catalysis, see: Dunina et al. (2008[Dunina, V. V., Turubanova, E. I., Livantsov, M. V., Lyssenko, K. A. & Grishin, Y. K. (2008). Tetrahedron Asymmetry 19, 1519-1522.], 2009[Dunina, V. V., Zykov, P. A., Livantsov, M. V., Glukhov, I. V., Kochetkov, K. A., Gloriozov, I. P. & Grishin, Y. K. (2009). Organometallics, 28, 425-432.]); Bedford et al. (2004[Bedford, R. B., Cazin, C. S. J. & Holder, D. (2004). Coord. Chem. Rev. 248, 2283-2321.]); Morales-Morales et al. (2002[Morales-Morales, D., Cramer, R. E. & Jensen, C. M. (2002). J. Organomet. Chem. 654, 44-50.]). For the synthesis of the starting materials, see: Drew & Doyle (1990[Drew, D. & Doyle, J. R. (1990). Inorg. Synth. 28, 346-349.]).

[Scheme 1]

Experimental

Crystal data
  • [Pd2(C30H20P)2Cl2]·2CH2Cl2

  • Mr = 1276.41

  • Triclinic, [P \overline 1]

  • a = 9.4823 (8) Å

  • b = 11.4272 (9) Å

  • c = 12.343 (1) Å

  • [alpha] = 80.652 (2)°

  • [beta] = 76.592 (2)°

  • [gamma] = 89.013 (2)°

  • V = 1283.42 (18) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 1.12 mm-1

  • T = 100 K

  • 0.33 × 0.13 × 0.13 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 = 0.709, Tmax = 0.868

  • 40200 measured reflections

  • 6340 independent reflections

  • 5675 reflections with I > 2[sigma](I)

  • Rint = 0.030

Refinement
  • R[F2 > 2[sigma](F2)] = 0.052

  • wR(F2) = 0.154

  • S = 1.07

  • 6340 reflections

  • 325 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.59 e Å-3

  • [Delta][rho]min = -2.36 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

Cg1, Cg2, Cg3 and Cg4 are the centroids of the C11-C15/C20, C21-C25/C30, Pd1/Cl1/Pd1'/Cl1' and C1/C2/C7-C10 rings, respectively.

D-H...A D-H H...A D...A D-H...A
C10-H10...Cl3 0.95 2.72 3.536 (7) 145
C31-H31A...Cl3i 0.99 2.52 3.366 (16) 143
C9-H9...Cg1ii 0.95 2.83 3.666 (5) 148
C18-H18...Cg2iii 0.95 2.91 3.788 (6) 154
C26-H26...Cg3iv 0.95 2.59 3.535 (5) 172
C31-H31B...Cg4ii 0.99 2.75 3.632 (15) 148
Symmetry codes: (i) -x, -y+1, -z; (ii) -x+1, -y+1, -z; (iii) x+1, y, z; (iv) -x, -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: ZQ2190 ).


Acknowledgements

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

References

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.
Drew, D. & Doyle, J. R. (1990). Inorg. Synth. 28, 346-349.  [CrossRef] [ChemPort]
Dunina, V. V., Turubanova, E. I., Livantsov, M. V., Lyssenko, K. A. & Grishin, Y. K. (2008). Tetrahedron Asymmetry 19, 1519-1522.  [CrossRef] [ChemPort]
Dunina, V. V., Zykov, P. A., Livantsov, M. V., Glukhov, I. V., Kochetkov, K. A., Gloriozov, I. P. & Grishin, Y. K. (2009). Organometallics, 28, 425-432.  [CrossRef] [ChemPort]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Morales-Morales, D., Cramer, R. E. & Jensen, C. M. (2002). J. Organomet. Chem. 654, 44-50.  [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]


Acta Cryst (2012). E68, m1565-m1566   [ doi:10.1107/S1600536812048222 ]

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