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Volume 69 
Part 3 
Pages m139-m140  
March 2013  

Received 25 January 2013
Accepted 29 January 2013
Online 6 February 2013

Key indicators
Single-crystal X-ray study
T = 298 K
Mean [sigma](C-C) = 0.006 Å
Disorder in main residue
R = 0.048
wR = 0.110
Data-to-parameter ratio = 16.2
Details
Open access

Chlorido[2,3,5,6-tetrakis(tert-butylsulfanylmethyl)phenyl-[kappa]3S2,C1,S6]palladium(II) dichloromethane monosolvate

aInstituto de Química, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, Coyoacan, CP 04510, México, DF, Mexico
Correspondence e-mail: evelynpm@unam.mx

The title compound, [Pd(C26H45S4)Cl]·CH2Cl2, crystallizes with a disordered dichloromethane solvent molecule [occupancy ratio = 0.67 (4):0.33 (4)]. Two of the tert-butyl groups are also disordered [occupancy ratios = 0.70 (5):0.30 (5) and 0.63 (4):0.37 (4)]. Although the pincer ligand offers the possibility for coordination of two different metal atoms, the present structure shows only the coordination of a single PdII atom in a typical S-C-S tridentate pincer manner. The PdII atom is in a slightly distorted square-planar environment with the two tert-butylsulfanyl groups arranged in a trans conformation and with a chloride ligand trans to the [sigma]-bonded aromatic C atom. The structure exhibits a durene-like ligand frame, forming a dihedral angle of 13.6 (4)° with the metal coordination (Pd/S/S/Cl/C) environment. It is noteworthy that the tert-butyl groups are found in a syn arrangement, this being different to that found previously by Loeb, Shimizu & Wisner [(1998). Organometallics, 17, 2324-2327].

Related literature

For background to pincer compounds, see: Arroyo et al., (2003[Arroyo, M., Cervantes, R., Gómez-Benitez, V., López, P., Morales-Morales, D., Torrens, H. & Toscano, R. A. (2003). Synthesis, pp. 1565-1568.]); Errington, et al. (1980[Errington, J., McDonald, W. S. & Shaw, B. L. (1980). J. Chem. Soc. Dalton Trans. pp. 2312-2314.]); Morales-Morales & Jensen (2007[Morales-Morales, D. & Jensen, C. M. (2007). In The Chemistry of Pincer Compounds. Amsterdam: Elsevier.]). For an isomeric structure, see: Loeb et al. (1998[Loeb, S. J., Shimizu, K. H. G. & Wisner, J. A. (1998). Organometallics, 17, 2324-2327.]).

[Scheme 1]

Experimental

Crystal data
  • [Pd(C26H45S4)Cl]·CH2Cl2

  • Mr = 712.64

  • Monoclinic, P 21 /n

  • a = 15.917 (15) Å

  • b = 13.768 (13) Å

  • c = 17.808 (16) Å

  • [beta] = 105.216 (15)°

  • V = 3766 (6) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 0.94 mm-1

  • T = 298 K

  • 0.27 × 0.22 × 0.15 mm

Data collection
  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: integration (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.593, Tmax = 0.745

  • 28207 measured reflections

  • 6570 independent reflections

  • 5144 reflections with I > 2[sigma](I)

  • Rint = 0.066

Refinement
  • R[F2 > 2[sigma](F2)] = 0.048

  • wR(F2) = 0.110

  • S = 1.03

  • 6570 reflections

  • 406 parameters

  • 291 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.64 e Å-3

  • [Delta][rho]min = -0.24 e Å-3

Table 1
Selected bond lengths (Å)

Pd-C2 2.022 (4)
Pd-S1 2.326 (2)
Pd-S2 2.333 (2)
Pd-Cl1 2.441 (2)

Data collection: SMART (Bruker, 1999[Bruker (1999). SMART and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 1999[Bruker (1999). SMART and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PK2463 ).


Acknowledgements

EPM would like to thank CONACYT for a postdoctoral scholarship (postdoctoral agreement No. 290662 UNAM). The financial support of this research by CONACYT (CB2010-154732) and DGAPA-UNAM (IN201711) is gratefully acknowledged. SHO would like to thank the Consejo Superior de Investigaciones Científicas (CSIC) of Spain for the award of a licence for the use of the Cambridge Structural Database.

References

Arroyo, M., Cervantes, R., Gómez-Benitez, V., López, P., Morales-Morales, D., Torrens, H. & Toscano, R. A. (2003). Synthesis, pp. 1565-1568.  [ISI] [CSD] [CrossRef]
Bruker (1999). SMART and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.
Errington, J., McDonald, W. S. & Shaw, B. L. (1980). J. Chem. Soc. Dalton Trans. pp. 2312-2314.  [CrossRef]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Loeb, S. J., Shimizu, K. H. G. & Wisner, J. A. (1998). Organometallics, 17, 2324-2327.  [CrossRef] [ChemPort]
Morales-Morales, D. & Jensen, C. M. (2007). In The Chemistry of Pincer Compounds. Amsterdam: Elsevier.
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]


Acta Cryst (2013). E69, m139-m140   [ doi:10.1107/S1600536813003036 ]

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