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Volume 69 
Part 7 
Pages m360-m361  
July 2013  

Received 24 May 2013
Accepted 28 May 2013
Online 8 June 2013

Key indicators
Single-crystal X-ray study
T = 153 K
Mean [sigma](C-C) = 0.005 Å
Disorder in main residue
R = 0.041
wR = 0.104
Data-to-parameter ratio = 18.0
Details
Open access

Bis{[2,2'-(5,8,11-trithia-2,14-diazapentadeca-1,14-diene-1,15-diyl)diphenolato]palladium(II)} acetonitrile monosolvate

aDepartment of Chemistry, Memorial University of Newfoundland, St John's, NL, A1B 3X7, Canada, and bC-CART X-Ray Diffraction Lab, Memorial University of Newfoundland, St John's, NL, A1B 3X7, Canada
Correspondence e-mail: louise.dawe@mun.ca

The asymmetric unit of the title compound, [Pd(C22H26N2O2S3)]2·CH3CN, contains two complex molecules and a single uncoordinated lattice acetonitrile solvent molecule. The PdII cations have a trans-N2O2 square-planar geometry and the superposition of the two crystallographically independent PdII complexes yields an overall r.m.s. deviation of 0.292 Å. The Pd...Pd separation in the asymmetric unit is 3.3776 (3) Å, while the PdN2O2 plane-plane fold angle is 1.62 (7)°. A short intermolecular S...S contact between the central S atom of one complex and its inversion-related symmetry equivalent of 3.663 (2) Å is observed. Part of the ligand chain (S-C-C-S) in each complex molecule is disordered over two orientations and refined occupancies that converged to 0.450 (10) and 0.550 (10) for the one complex molecule, and 0.789 (9) and 0.211 (9) for the other.

Related literature

For the synthesis of the ligand 5,8,11-trithia-2,14-diazapentadeca-1,14-diene-1,15-diyl)diphenolate, and the related complexes [2,2'-(5,8-dithia-2,11-diazododeca-1,11-diene-1,12-diyl)diphenolato]cobalt tetrafluoroborate and [2,2'-(5,8-dithia-2,11-diazododeca-1,11-diene-1,12-diyl)diphenolato]nickel acetate, see: Lucas et al. (2011a[Lucas, C. R., Byrne, J. M. D., Collins, J. L., Dawe, L. N. & Miller, D. O. (2011a). Can. J. Chem. 89, 1174-1189.]). For the preparation of the starting material, bis(acetonitrile)dichloropalladium(II), from which the title complex was synthesized, see: Mathews et al. (2003[Mathews, C. J., Smith, P. J. & Welton, T. (2003). J. Mol. Catal. A Chem. 206, 77-82.]). For a copper complex containing the same ligand as the title complex, bis[[mu]2-2,2'-(5,8,11-trithia-2,14-diazapentadeca-1,14-diene-1,15-diyl)diphenolato]dicopper(II), see: Lucas et al. (2011b[Lucas, C. R., Byrne, J. M. D., Collins, J. L., Dawe, L. N. & Miller, D. O. (2011b). Can. J. Chem. 89, 1190-1201.]). Lucas et al. (2011b[Lucas, C. R., Byrne, J. M. D., Collins, J. L., Dawe, L. N. & Miller, D. O. (2011b). Can. J. Chem. 89, 1190-1201.]) also reports the related [2,2'-(5,8-dithia-2,11-diazadodeca-1,11-diene-1,12-diyl)diphenolato]copper(II). For Pd catalysts containing salicylaldimine (sal) ligands, see: Jin et al. (2010[Jin, Z., Qiu, L.-L., Li, Y.-Q., Hong, H.-B. & Fang, J.-X. (2010). Organometallics, 29, 6578-6586.]). For a discussion on the coordination capabilities of PdII, see: Aullón & Alvarez (1996[Aullón, G. & Alvarez, S. (1996). Inorg. Chem. 35, 3137-3144.]). For a description of the Cambridge Crystallographic Database, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]).

[Scheme 1]

Experimental

Crystal data
  • [Pd(C22H26N2O2S3)]2·C2H3N

  • Mr = 1147.11

  • Monoclinic, P 21 /c

  • a = 14.7232 (5) Å

  • b = 16.2151 (5) Å

  • c = 20.9433 (8) Å

  • [beta] = 106.087 (1)°

  • V = 4804.2 (3) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.06 mm-1

  • T = 153 K

  • 0.39 × 0.39 × 0.24 mm

Data collection
  • Rigaku Saturn70 diffractometer

  • Absorption correction: numerical (ABSCOR; Higashi, 2000[Higashi, T. (2000). ABSCOR. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.794, Tmax = 0.862

  • 53768 measured reflections

  • 10948 independent reflections

  • 10673 reflections with I > 2[sigma](I)

  • Rint = 0.025

Refinement
  • R[F2 > 2[sigma](F2)] = 0.041

  • wR(F2) = 0.104

  • S = 1.07

  • 10948 reflections

  • 607 parameters

  • 74 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 1.16 e Å-3

  • [Delta][rho]min = -1.02 e Å-3

Data collection: CrystalClear (Rigaku, 2005[Rigaku (2005). Rigaku/AFC Diffractometer Control Software. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: Mercury (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.]) and ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]) and publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HG5318 ).


Acknowledgements

Financial assistance from the Memorial University of Newfoundland is acknowledged.

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.  [Web of Science] [CrossRef] [IUCr Journals]
Aullón, G. & Alvarez, S. (1996). Inorg. Chem. 35, 3137-3144.  [PubMed]
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Higashi, T. (2000). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Jin, Z., Qiu, L.-L., Li, Y.-Q., Hong, H.-B. & Fang, J.-X. (2010). Organometallics, 29, 6578-6586.  [CSD] [CrossRef] [ChemPort]
Lucas, C. R., Byrne, J. M. D., Collins, J. L., Dawe, L. N. & Miller, D. O. (2011a). Can. J. Chem. 89, 1174-1189.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Lucas, C. R., Byrne, J. M. D., Collins, J. L., Dawe, L. N. & Miller, D. O. (2011b). Can. J. Chem. 89, 1190-1201.  [Web of Science] [CSD] [CrossRef] [ChemPort]
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.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Mathews, C. J., Smith, P. J. & Welton, T. (2003). J. Mol. Catal. A Chem. 206, 77-82.  [Web of Science] [CrossRef] [ChemPort]
Rigaku (2005). Rigaku/AFC Diffractometer Control Software. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]


Acta Cryst (2013). E69, m360-m361   [ doi:10.1107/S1600536813014712 ]

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