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Volume 68 
Part 12 
Page m1502  
December 2012  

Received 19 October 2012
Accepted 14 November 2012
Online 17 November 2012

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.004 Å
R = 0.020
wR = 0.045
Data-to-parameter ratio = 23.7
Details
Open access

Bis[O-isopropyl (4-ethoxyphenyl)dithiophosphonato-[kappa]2S,S']lead(II)

aSchool of Chemistry and Physics, University of KwaZulu-Natal, Westville Campus, Private Bag X54001, Durban 4000, South Africa
Correspondence e-mail: vanzylw@ukzn.ac.za

The title compound, [Pb(C11H16O2PS2)2], is a neutral four-coordinate mononuclear complex with a distorted square-pyramidal geometry of the PbS4 core. The apical PbII atom of each pyramid is 1.33059 (3) Å above the basal S4 plane. The metal atom is surrounded by two chelating dithiophosphonate ligands binding through the S-donor atoms. The ligands are anisobidentate as the pyramid is comprised of Pb-S bond lengths that vary substantially [2.6999 (7), 2.7128 (6), 2.8877 (7) and 2.9472 (7) Å], clearly indicating two short and two longer bond lengths. The P-S bond lengths are also paired as shorter [1.9959 (9) and 1.9877 (8) Å] and slightly longer [2.0115 (9) and 2.0245 (9) Å], indicating an anisobidentate nature of the ligand whereby the shorter P-S bond has more double-bond character than the other. The S-Pb-S (chelating) bond angles range from 71.841 (18) to 72.692 (19)°, whilst the Pb-S-P bond angles range from 84.70 (3) to 90.51 (3)°.

Related literature

For information on dithiophosphonate compounds, see: Van Zyl & Fackler (2000[Van Zyl, W. E. & Fackler, J. P. (2000). Phosphorus Sulfur Silicon Relat. Elem. 167, 117-132.]); Van Zyl (2010[Van Zyl, W. E. (2010). Comments Inorg. Chem. 31, 13-45.]). For similar lead(II) dithiophosphonate complexes, see: Gray et al. (2003[Gray, I. P., Milton, H. L., Slawin, A. M. Z. & Woollins, J. D. (2003). Dalton Trans. pp. 3450-3457.], 2004[Gray, I. P., Slawin, A. M. Z. & Woollins, J. D. (2004). Dalton Trans. pp. 2477-2486.]).

[Scheme 1]

Experimental

Crystal data
  • [Pb(C11H16O2PS2)2]

  • Mr = 757.85

  • Triclinic, [P \overline 1]

  • a = 10.2092 (8) Å

  • b = 11.7016 (10) Å

  • c = 12.9915 (10) Å

  • [alpha] = 89.297 (2)°

  • [beta] = 85.016 (2)°

  • [gamma] = 69.034 (1)°

  • V = 1443.5 (2) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 6.27 mm-1

  • T = 173 K

  • 0.16 × 0.14 × 0.11 mm

Data collection
  • Bruker Kappa DUO APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.434, Tmax = 0.546

  • 36710 measured reflections

  • 7212 independent reflections

  • 6564 reflections with I > 2[sigma](I)

  • Rint = 0.037

Refinement
  • R[F2 > 2[sigma](F2)] = 0.020

  • wR(F2) = 0.045

  • S = 1.03

  • 7212 reflections

  • 304 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.61 e Å-3

  • [Delta][rho]min = -0.63 e Å-3

Data collection: APEX2 (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: GK2529 ).


Acknowledgements

The authors thank the National Research Foundation (NRF) and UKZN for financial support.

References

Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Gray, I. P., Milton, H. L., Slawin, A. M. Z. & Woollins, J. D. (2003). Dalton Trans. pp. 3450-3457.  [CSD] [CrossRef]
Gray, I. P., Slawin, A. M. Z. & Woollins, J. D. (2004). Dalton Trans. pp. 2477-2486.  [CSD] [CrossRef]
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Van Zyl, W. E. (2010). Comments Inorg. Chem. 31, 13-45.  [ISI] [CrossRef] [ChemPort]
Van Zyl, W. E. & Fackler, J. P. (2000). Phosphorus Sulfur Silicon Relat. Elem. 167, 117-132.  [CrossRef] [ChemPort]


Acta Cryst (2012). E68, m1502  [ doi:10.1107/S1600536812046818 ]

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