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Volume 69 
Part 1 
Pages m29-m30  
January 2013  

Received 16 November 2012
Accepted 21 November 2012
Online 8 December 2012

[bt6859sup1]
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Key indicators
Single-crystal X-ray study
T = 123 K
Mean [sigma](C-C) = 0.012 Å
Disorder in main residue
R = 0.030
wR = 0.075
Data-to-parameter ratio = 11.1
Details
Open access

catena-Poly[[[O,O'-bis(2-methylphenyl) dithiophosphato-[kappa]2S,S]lead(II)]-[mu]-O,O'-bis(2-methylphenyl) dithiophosphato-[kappa]3S,S':S]

Ray J. Butcher,a* Raju Ratnani,b+ Sema Öztürk Yildirima,c and Oluwaseun Falolaa

aDepartment of Chemistry, Howard University, 525 College Street NW, Washington, DC 20059, USA,bDepartment of Pure & Applied Chemistry, M.D.S. University, Ajmer 305 009, India, and cDepartment of Physics, Faculty of Sciences, Erciyes University, 38039 Kayseri, Turkey
Correspondence e-mail: rbutcher99@yahoo.com

In the title compound, [Pb(C14H14O2PS2)2]n, the metal atom is surrounded by two O,O'-bis(2-methylphenyl) dithiophosphate ligands bonding through the S-donor atoms. Three of the Pb-S bond lengths are are close to each other at 2.7710 (18), 2.8104 (16) and 2.8205 (16) Å, while the fourth Pb-S bond is elongated at 3.0910 (18) Å and reflects the fact that this atom is involved in intermolecular bridging to an adjacent PbII atom [Pb-S = 3.145 (2) Å]. The bond angles demonstrate that the PbII atom contains a stereochemically active lone pair with a distorted octahedral geometry about the PbII atom. This distortion is shown by the S-Pb-S bite angles of 73.63 (4) and 69.50 (4)°, while the remaining S-Pb-S angles range from 81.03 (5) to 143.66 (5)°. One of the benzene rings shows positional disorder over two orientations with occupancy factors of 0.747 (11) and 0.253 (11).

Related literature

For applications of related O,O'-dialkyl derivatives of phosphorus(V) dithioacids, see: Lawton & Kokotailo (1969[Lawton, S. L. & Kokotailo, G. T. (1969). Nature (London), 221, 550-551.], 1972[Lawton, S. L. & Kokotailo, G. T. (1972). Inorg. Chem. 11, 363-368.]); Ito (1972[Ito, T. (1972). Acta Cryst. B28, 1034-1040.]); Harrison et al. (1988[Harrison, Ph. G., Steel, A., Pelizzi, G. & Pellizi, C. (1988). Main Group Met. Chem. 11, 181-204.]). For general and convenient methods for the preparation of dithiophosphato salt derivatives and their metal derivatives, see: Bajia et al. (2009[Bajia, S., Butcher, R. J., Drake, J. E. & Ratnani, R. (2009). Polyhedron, 28, 1556-1560.]); Maheshwari et al. (2009[Maheshwari, S., Drake, J. E., Kori, K., Light, M. E. & Ratnani, R. (2009). Polyhedron, 28, 689-694.]); Lawton & Kokotailo (1969[Lawton, S. L. & Kokotailo, G. T. (1969). Nature (London), 221, 550-551.], 1972[Lawton, S. L. & Kokotailo, G. T. (1972). Inorg. Chem. 11, 363-368.]); Ito (1972[Ito, T. (1972). Acta Cryst. B28, 1034-1040.]); Harrison et al. (1988[Harrison, Ph. G., Steel, A., Pelizzi, G. & Pellizi, C. (1988). Main Group Met. Chem. 11, 181-204.]); 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 VSEPR theory, see: Gillespie & Nyholm (1957[Gillespie, R. J. & Nyholm, R. S. (1957). Q. Rev. 11, 339-380.]). For stereochemically active lone pairs in Pb2+ complexes, see: Davidovich et al. (2010[Davidovich, R. L., Stavila, V. & Whitmire, K. H. (2010). Coord. Chem. Rev. 254, 2193-2226.]); Ito & Maeda (2004[Ito, T. & Maeda, Y. (2004). Acta Cryst. E60, m1349-m1350.]); Larsson et al. (2004[Larsson, A.-C., Ivanov, A. V., Antzutkin, O. N., Gerasimenko, A. V. & Forsling, W. (2004). Inorg. Chim. Acta, 357, 2510-2518.]); Lawton & Kokotailo (1972[Lawton, S. L. & Kokotailo, G. T. (1972). Inorg. Chem. 11, 363-368.]).

[Scheme 1]

Experimental

Crystal data

  • [Pb(C14H14O2PS2)2]

  • Mr = 825.87

  • Monoclinic, P 21

  • a = 12.0263 (6) Å

  • b = 10.7420 (4) Å

  • c = 13.0499 (8) Å

  • [beta] = 112.849 (6)°

  • V = 1553.58 (15) Å3

  • Z = 2

  • Cu K[alpha] radiation

  • [mu] = 14.31 mm-1

  • T = 123 K

  • 0.46 × 0.05 × 0.03 mm
Data collection

  • Agilent Xcalibur (Ruby, Gemini) diffractometer

  • Absorption correction: analytical [CrysAlis PRO (Agilent, 2011[Agilent (2011). CrysAlis PRO and CrysAlis RED. Agilent Technologies, Yarnton, England.]), using a multi-faceted crystal model (Clark & Reid, 1995[Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.])] Tmin = 0.094, Tmax = 0.675

  • 10226 measured reflections

  • 4494 independent reflections

  • 4269 reflections with I > 2[sigma](I)

  • Rint = 0.045
Refinement

  • R[F2 > 2[sigma](F2)] = 0.030

  • wR(F2) = 0.075

  • S = 1.03

  • 4494 reflections

  • 406 parameters

  • 55 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 1.12 e Å-3

  • [Delta][rho]min = -1.15 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1093 Friedel pairs

  • Flack parameter: -0.03 (8)

Data collection: CrysAlis PRO (Agilent, 2011[Agilent (2011). CrysAlis PRO and CrysAlis RED. Agilent Technologies, Yarnton, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; 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: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BT6859 ).

Acknowledgements

RJB acknowledges the NSF-MRI program (grant No. CHE-0619278) for funds to purchase the diffractometer.

References

Agilent (2011). CrysAlis PRO and CrysAlis RED. Agilent Technologies, Yarnton, England.
Bajia, S., Butcher, R. J., Drake, J. E. & Ratnani, R. (2009). Polyhedron, 28, 1556-1560.  [ISI] [CSD] [CrossRef] [ChemPort]
Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.  [CrossRef] [details]
Davidovich, R. L., Stavila, V. & Whitmire, K. H. (2010). Coord. Chem. Rev. 254, 2193-2226.  [ISI] [CrossRef] [ChemPort]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Gillespie, R. J. & Nyholm, R. S. (1957). Q. Rev. 11, 339-380.  [CrossRef] [ChemPort]
Harrison, Ph. G., Steel, A., Pelizzi, G. & Pellizi, C. (1988). Main Group Met. Chem. 11, 181-204.  [ChemPort]
Ito, T. (1972). Acta Cryst. B28, 1034-1040.  [CrossRef] [ChemPort] [details] [ISI]
Ito, T. & Maeda, Y. (2004). Acta Cryst. E60, m1349-m1350.  [CrossRef] [details]
Larsson, A.-C., Ivanov, A. V., Antzutkin, O. N., Gerasimenko, A. V. & Forsling, W. (2004). Inorg. Chim. Acta, 357, 2510-2518.  [ISI] [CSD] [CrossRef] [ChemPort]
Lawton, S. L. & Kokotailo, G. T. (1969). Nature (London), 221, 550-551.  [CrossRef] [ChemPort] [ISI]
Lawton, S. L. & Kokotailo, G. T. (1972). Inorg. Chem. 11, 363-368.  [CrossRef] [ChemPort] [ISI]
Maheshwari, S., Drake, J. E., Kori, K., Light, M. E. & Ratnani, R. (2009). Polyhedron, 28, 689-694.  [ISI] [CSD] [CrossRef] [ChemPort]
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 (2013). E69, m29-m30   [ doi:10.1107/S1600536812047964 ]

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